CN108872456B - Column oven for gas chromatograph and gas chromatograph apparatus using the same - Google Patents

Column oven for gas chromatograph and gas chromatograph apparatus using the same Download PDF

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CN108872456B
CN108872456B CN201710757198.1A CN201710757198A CN108872456B CN 108872456 B CN108872456 B CN 108872456B CN 201710757198 A CN201710757198 A CN 201710757198A CN 108872456 B CN108872456 B CN 108872456B
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metal plate
column oven
column
plate member
gas chromatograph
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CN108872456A (en
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冈田昌之
涉谷龙太
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Shimadzu Corp
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Shimadzu Corp
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/26Conditioning of the fluid carrier; Flow patterns
    • G01N30/28Control of physical parameters of the fluid carrier
    • G01N30/30Control of physical parameters of the fluid carrier of temperature
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/60Construction of the column

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
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  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Investigating Or Analyzing Materials Using Thermal Means (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Baking, Grill, Roasting (AREA)

Abstract

The invention provides a column oven for a gas chromatograph and a gas chromatograph using the same, which can reliably reduce the explosion scale even if the flammable gas reserved in the column oven chamber body is ignited. The column oven chamber body of a substantially rectangular parallelepiped shape housing the column is formed by fitting and screwing a plurality of metal plate members of a substantially flat plate shape, a substantially L shape, or a substantially Contraband shape without welding. Further, in the opening of the front surface opened and closed by the door, a front frame metal plate member having a substantially frame shape is attached to the outer 1 st metal plate member by the same method. Since the corner portions extending in the Y direction on the left and right upper sides of the column oven chamber main body and the attachment portions of the front frame metal plate member and the outer 1 st metal plate member are lower in strength than the other portions, when the air pressure in the internal space rises to a certain extent due to explosion, breakage, fracture, or deformation occurs, and an opening is formed. Gas will flow out through the opening to reduce the size of the explosion.

Description

Column oven for gas chromatograph and gas chromatograph apparatus using the same
Technical Field
The present invention relates to a column oven for a Gas Chromatograph (GC) for adjusting the temperature of a column for the gas chromatograph, and a gas chromatograph apparatus using the same.
Background
In a gas chromatography apparatus, a gaseous sample is introduced into a column with a flow of a carrier gas, and various compounds in the sample are separated in a time direction while the sample passes through the column. Then, the sample gas discharged from the outlet end of the column is introduced into a detector, and the compounds contained in the sample gas are sequentially detected in the detector. The column is housed in a column oven for gas chromatograph (hereinafter, simply referred to as "column oven") for temperature adjustment, and during the execution of analysis, the column is fixedly maintained at a predetermined temperature by the column oven or adjusted so that the temperature rises with the passage of time according to a predetermined temperature rise program.
The column oven is generally configured by providing a heater and a fan inside a substantially rectangular parallelepiped column oven chamber having an internal space of a size capable of accommodating a column, and a large opening for taking and placing the column provided on a front surface of the column oven chamber is opened and closed by a side-opening door. In general, in order to improve the performance of temperature adjustment, the column temperature chamber is configured to maintain high airtightness in a state where the door is closed.
In a gas chromatography apparatus, hydrogen gas is sometimes used as a carrier gas. In addition, in a gas chromatography apparatus, a detector that requires hydrogen gas for detection, such as a hydrogen Flame Ionization Detector (FID), may be used. In this case, if a connection failure occurs in a connection portion between the column and the sample introduction portion, a connection portion between the column and the detection portion, or the like, or if the column or the connection device has a defect or is damaged, hydrogen gas leaks out and accumulates in the column oven chamber in a sealed state. If the accumulated hydrogen gas is ignited by some cause such as heat or static electricity from the heater, explosion may occur, and the components of the column oven may be scattered around (see non-patent document 1 and the like). As a column oven that employs a countermeasure against such an explosion, there is a column oven described in patent document 1.
Fig. 7 (a) is a schematic horizontal cross-sectional view of the column oven described in patent document 1 (in which some elements are shown as end faces in order to avoid complication of the drawing). In the figure, the surface facing downward is the front surface, and the surface facing upward is the back surface.
The column oven includes a column oven main body 200 having a substantially rectangular parallelepiped shape with the entire front surface thereof opened, and a door 213 that opens and closes an opening in the front surface of the column oven main body 200, and when the door 213 is closed, an internal space 218 for accommodating a column is formed. The column oven chamber main body 200 is constituted by a right side wall 201, a left side wall 202, a back wall 203, and a bottom wall 204 as seen in fig. 7 (a), and a top wall not appearing in fig. 7 (a). Each wall has a 3-layer structure in which a heat insulating material such as glass wool is sandwiched between 2 metal plates. A motor 210 is attached to the rear wall 203, and a fan 211 is fixed to a rotating shaft of the motor 210 extending to the internal space 218. Further, a heater 212 is disposed so as to surround the fan 211.
The door 213 includes a door main body 2131, an inner door 2132 made of a heat insulating material such as glass wool, and a spring 2133 for urging the inner door 2132 against the door main body 2131 toward the internal space 218. The door main body 2131 is fixed to the column oven chamber main body 200 (strictly, the left side wall 202) so as to be rotatable about a door shaft 214 extending in the vertical direction (in fig. 7 a, the direction perpendicular to the paper surface). As shown in fig. 7 (a), when the door 213 is closed, the inner door 2132 is pushed rearward by the biasing force of the spring 2133. Thus, the inner door 2132 is pressed against the front edge portions of the upper, lower, left, and right side walls 201, 202, and the like, and the door 213 substantially seals the column-temperature box main body 200.
A substantially L-shaped latch 215 is rotatably attached to a right end portion of the door main body 2131 (i.e., an end portion on the opposite side of the door shaft 214) about a latch shaft 216 extending in the vertical direction. A hook portion 217 having a shape to engage with the hook portion of the latch 215 is fixed to the column oven chamber main body 200 (strictly, the right side wall 201). Although not shown, the latch 215 is urged counterclockwise in fig. 7 (a) by a spring, and as shown in fig. 7 (a), in a state where the door 213 is closed so as to close the front surface opening of the column oven chamber main body 200, the hook portion of the latch 215 is engaged with the hook portion 217, so that the door 213 is reliably held in the closed state. In the case of opening the door 213, the user grips a handle, not shown, at the front surface of the door 213. Then, the engagement of the hook portion of the latch 215 with the hook portion 217 is temporarily released, so that the user can open the door 213 forward.
As described above, when the door 213 is closed and the internal space 218 is substantially sealed, if hydrogen gas is accumulated in the internal space 218 and ignited, an explosion occurs. Then, the air pressure rises sharply in the internal space 218. As described above, the inner door 2132 is pressed rearward by the spring 2133, but since the rapidly rising air pressure is stronger than the pressing force of the spring 2133, the inner door 2132 is pressed by the air pressure and approaches the door main body 2131 as indicated by the hollow arrow in fig. 7 (b). Then, a gap is formed between the inner door 2132 and the front edges of the left and right side walls 201 and 202, and the gas is ejected from the internal space 218 through the gap. Namely, a kind of exhaust is performed through the gap. This alleviates the increase in the air pressure in the internal space 218, and reduces the size of the explosion.
However, the conventional column oven has the following problems.
As described above, when the gas is rapidly discharged through the gap between the inner door 2132 and the front edge portions of the left and right side walls 201 and 202, the momentum of the gas flow is extremely large. When the airflow hits the latch 215 at the right end of the door 213, the latch 215 receives a large force in the direction indicated by the arrow in fig. 7 (b), and the hook portion may be disengaged from the hook portion 217. Thus, the door 213 is pushed by the air pressure applied to the entire inner door 2132 and suddenly opened, and there is a risk of contact with a user located in front of the door 213.
In the conventional column oven, although a part of the gas flows out through the gap between the inner door 2132 and the front edge portions of the left and right side walls 201 and 202, the gas does not necessarily flow out in a large amount, and therefore, the gas in the internal space 218 explodes in a state where the gas pressure is considerably high. As a result, the size of the explosion is often large. Therefore, the members constituting the column oven may suddenly scatter around, and such scattered objects may cause personal injury and property loss.
[ Prior art documents ]
[ patent document ]
[ patent document 1 ] Japanese patent laid-open No. 2016-217912 publication
[ patent document 2 ] Japanese patent laid-open No. 2002-14087 (paragraph [0003])
[ non-patent literature ]
[ non-patent document 1 ] regarding safe use of hydrogen gas (note on use) 6. risk to be assumed when gas chromatograph is operated, "online, manufactured by shimadzu corporation, [ online ], [ search 4/28/2017 ], website < URL: http:// www.an.shimadzu.co.jp/gc/support/faq/bombe6.htm > ("water ガス is safely used について (note on the front wall) 6.ガス ク ロ マ ト グ ラ フ political fragment に imagines される dangerous ", zhui zhenju zhijun mo (in 29 years 4 and 28 days), インターネット < URL: http:// www.an.shimadzu.co.jp/support/faq/bombe6. htm >)
Disclosure of Invention
[ problem to be solved by the invention ]
Since the explosion is caused by improper use of the apparatus or a defect of the apparatus, it is not possible to damage the apparatus itself including the column oven, but it is naturally preferable to suppress the damage to the property and the injury to the person of the facility in which the apparatus is installed as much as possible.
The present invention has been made to solve the above problems, and an object of the present invention is to provide a column oven for a gas chromatograph and a gas chromatograph apparatus using the same, in which: even if a combustible gas such as hydrogen gas accumulated in the internal space of the column oven is ignited and explodes, the scale of the explosion can be suppressed and personal injury and property loss can be reliably reduced.
[ MEANS FOR SOLVING PROBLEMS ] A method for producing a semiconductor device
Generally, a column oven chamber main body of a column oven for a gas chromatograph is assembled into a box shape by welding a metal thin plate such as a stainless plate (see patent document 2). With such a structure, the column oven chamber main body has high sealing performance and high strength, and is less likely to deform even if a force is applied from the outside, for example. However, when the above-described explosion occurs in the internal space of the column temperature chamber, if the tightness and the robustness of the column temperature chamber main body are high, the gas pressure becomes considerably high and the destruction occurs, and when the gas pressure rises to a level exceeding the breakdown pressure of the column temperature chamber, a large explosion occurs. That is, in the case of an explosion caused by ignition of the combustible gas accumulated in the column temperature chamber, the high airtightness and the high solidity of the column temperature chamber main body may be a factor causing a greater damage.
In general, as one of measures for preventing explosion of equipment and containers in which there is a risk of explosion such as dust collectors and coal bunkers, an explosion relief port (explosion venting port) is provided. The explosion relief port is as follows: the pressure vessel itself is ruptured under a predetermined pressure, and thus, an abnormal pressure generated by an explosion inside the apparatus or the vessel is rapidly released to the outside, thereby preventing or reducing the damage of the apparatus or the vessel. The present inventors have found that this explosion-proof method is effective also in a column oven for a gas chromatograph. The present inventors have also conceived the following to complete the present invention: the strength of a part of the column oven chamber main body is intentionally made weaker than that of the other part, and the relatively weak part is broken at a stage when the gas pressure at the initial stage of explosion is relatively low, so that an opening for dissipating the gas pressure to the outside is formed, thereby suppressing the scale of explosion.
That is, in order to solve the above-mentioned problems, a column oven for gas chromatograph according to the present invention includes a column oven chamber main body having a substantially rectangular parallelepiped shape and an opening on a front surface, and a door opening and closing the opening on the front surface of the column oven chamber main body, wherein an internal space for housing a chromatographic column is formed by the column oven chamber main body and the door,
the five wall surfaces of the right side surface, the left side surface, the bottom surface, the top surface and the back surface except the front surface of the column-temperature box chamber main body are formed by using at least 2 metal plate members bent in a shape of approximate Contraband or an approximate L shape or metal plate members in an approximate flat plate shape,
at least one of corner portions between adjacent two surfaces formed by abutting different metal plate members at substantially right angles to each other is provided as a drainage connecting portion formed by connecting two metal plate members by a method lower in strength than welding,
when the gas pressure in the internal space rises to a predetermined level or more, the vent connection part is detached, broken, or deformed, thereby forming an opening functioning as an explosion vent.
When a gas chromatograph column oven of the present invention is used to perform gas chromatography, the front opening of the column oven chamber main body in which the column is housed is closed by a door. If a combustible gas such as hydrogen gas is accumulated in the internal space in a substantially sealed state for some reason and is ignited by heat, static electricity, or the like from the heater, explosion occurs and the gas pressure in the internal space rises rapidly. When the air pressure rises to a certain extent, the pressure may cause the metal plate member at the connection portion for bleeding to detach, break, or deform, thereby forming an opening. Then, the gas flows out of the internal space through the opening, and thus a rapid increase in the gas pressure in the internal space is alleviated. As a result, the explosion is terminated on a relatively small scale, and the extent of the explosion can be sufficiently suppressed even when various members of the column oven chamber main body, the door, or members such as the heater and the fan disposed in the column oven chamber, and the chromatography apparatus main body in which the column oven chamber is incorporated, are broken and scattered.
In the column oven for gas chromatograph of the present invention, various methods can be used as the above-described "method of lower strength than welding". For example, a method of inserting a convex piece formed by bending one metal plate member at a substantially right angle into an insertion opening of the other metal plate member, a method of screwing a convex piece formed by bending one metal plate member at a substantially right angle to the other metal plate member, and the like can be cited. In the latter case, the width of the convex piece to be screwed is preferably made small. Thus, when the air pressure rises to a certain degree, not only the convex piece deforms under the pressure to cause the screw to fall off, but also the convex piece is easily broken.
In the column oven for a gas chromatograph of the present invention, five wall surfaces of a right side surface, a left side surface, a bottom surface, a top surface, and a back surface of a column oven chamber main body are respectively provided as a 3-layer structure in which a heat insulating material is interposed between 2 metal plates of an inner metal plate and an outer metal plate.
In this case, the five wall surfaces of the right side surface, the left side surface, the bottom surface, the top surface, and the back surface disposed inside (on the side of the internal space) the heat insulating material are formed by using at least 2 metal plate members bent in a substantially Contraband-shape or a substantially L-shape or substantially flat plate-shaped metal plate members, while the five wall surfaces of the right side surface, the left side surface, the bottom surface, the top surface, and the back surface disposed outside (on the side of the exterior) the heat insulating material are formed by using at least 2 metal plate members bent in a substantially Contraband-shape or a substantially L-shape or substantially flat plate-shaped metal plate members other than the at least 2 metal plate members. In this case, it is preferable that the substantially frame-shaped metal plate member is attached to the metal plate member forming the right side surface, the left side surface, the bottom surface, and the top surface so as to close between the end edges of the metal plate facing the inside and the outside of the front surface on the right side surface, the left side surface, the bottom surface, and the top surface, and the inner surface of the door is closely attached to the substantially frame-shaped metal plate member when the door is closed.
Further, a corner portion between two adjacent surfaces formed by the substantially frame-shaped metal plate member abutting substantially at right angles to the metal plate members forming the right side surface, the left side surface, the bottom surface, and the top surface is preferably a drainage connecting portion formed by connecting two metal plate members by a method lower in strength than welding.
In the column oven for gas chromatograph according to the present invention, it is preferable that: when the bent portion of the metal plate member bent in the substantially Contraband shape or the substantially L shape is the corner portion, a perforated linear portion is provided in which small holes are intermittently formed along the bent position.
The hole-line-shaped portion is more easily broken than a normal bent portion. Therefore, in the above preferred configuration, when the flammable gas accumulated in the internal space is ignited and explodes to increase the gas pressure in the internal space to a certain extent, the pressure causes the vent connection portion to break and also causes the holed linear portion to break, thereby facilitating deformation of the metal plate sandwiching the broken portion. This forms a large opening through which the gas flows out of the internal space, thereby further alleviating a rapid increase in the gas pressure in the internal space.
In the column oven for a gas chromatograph according to the present invention, it is preferable that: all corners except the bent portion are formed as a drainage connecting portion formed by connecting two metal plate members by a method having a lower strength than welding.
Since the column oven for a gas chromatograph has a large external size, it is common to build a final assembly factory in a place (country) close to a use area, and transport parts manufactured in other basic factories to the final assembly factory where the parts are assembled into a finished product. In the conventional structure in which the box-shaped column oven main body is assembled by welding, it is necessary to introduce welding equipment into a final assembly factory or to transport a box-shaped member manufactured in a basic factory to the final assembly factory. In the former case, the welding equipment is costly. On the other hand, in the latter case, the transportation cost of the box-like member having the cavity inside is high.
In contrast, in the column oven for gas chromatograph having the above configuration according to the present invention, the welding operation is not required in the manufacturing process of assembling the column oven chamber main body, and the column oven chamber main body can be assembled by fitting and screwing the plurality of metal plate members. Thus, no welding equipment has to be introduced in the final assembly plant. Further, the box-like member does not need to be transported to the final assembly plant, and any member capable of transporting a larger number of box-like members per the same volume, such as a substantially Contraband-shaped metal plate member, a substantially L-shaped bent metal plate member, or a substantially flat plate-like metal plate member, may be transported to the final assembly plant. Therefore, there is an advantage in that the cost of manufacturing equipment and the transportation cost of the members can be reduced.
In the column oven for a gas chromatograph according to the present invention, it is preferable that: at least a part of the connection for bleeding, which is formed by connecting two metal plate members by a method having a lower strength than welding, has a play between the two metal plate members.
According to this configuration, even when each of the metal plate members expands and contracts due to heat, the expansion and contraction is absorbed by the play between the two metal plate members, and therefore, it is possible to avoid an unreasonable load from being applied to the connecting portion. This prevents cracks from being generated in the conventional structure in which the metal plate members are connected to each other by welding, and high durability can be achieved.
Further, in the case where the five wall surfaces of the right side surface, the left side surface, the bottom surface, the top surface, and the back surface of the column oven chamber main body have a 3-layer structure as described above, the inner metal plate may reach an extremely high temperature (for example, about 450 ℃ at the maximum) when the column oven is used, whereas the outer metal plate is separated from the inner metal plate by the heat insulating material, and therefore, the temperature thereof is about 150 ℃ at the maximum. Therefore, the temperature difference between the inner metal plate and the outer metal plate with the heat insulating material interposed therebetween may be extremely large. In a configuration in which a substantially frame-shaped metal plate member is attached so as to block between the end edge portions of the metal plate facing the inside and the outside of the front surface on each of the right side surface, the left side surface, the bottom surface, and the top surface, a large temperature difference occurs between the inside and the outside of the substantially frame-shaped metal plate member, and a force due to thermal expansion and contraction concentrates particularly on the corners of the four corners on the inside, so that fatigue failure progresses, and cracks are likely to occur.
In particular, in a conventional column oven for a gas chromatograph, in order to weld a substantially frame-shaped metal plate member to a metal plate forming the inside of the right side surface, the left side surface, the bottom surface, and the top surface of the column oven chamber main body, the edge of the inside of the substantially frame-shaped metal plate member is bent at substantially right angles, and in this case, relief grooves (notches) are formed at the corners of the four corners. As described above, stress generated by expansion and contraction of the metal plate member due to a large temperature difference between the inside and the outside concentrates on the relief groove, and thus cracks are likely to be generated from the portion of the relief groove.
Therefore, the column oven for gas chromatograph according to the present invention is preferably configured as follows: the metal plate member having a substantially frame shape is bent backward at substantially right angles toward the linear portions of the four inner sides, and a corner portion between any 2 adjacent linear portions has a substantially circular arc shape in front view.
According to this configuration, even if there is expansion and contraction of the metal plate due to a large temperature difference between the inside and the outside of the substantially frame-shaped metal plate member, the stress generated by the expansion and contraction is appropriately dispersed without being concentrated on the corner portions of the four corners. Therefore, unlike a conventional column oven for a gas chromatograph, a metal plate member having a substantially frame shape is less likely to crack, and high durability can be achieved.
Further, the bent portions of the linear portions of the substantially frame-shaped metal plate member and the metal plate members on the inner sides of the right side surface, the left side surface, the bottom surface, and the top surface of the column oven chamber main body are connected by not welding, and for example, only the bent portions are pressed against the metal plate members on the inner sides of the right side surface, the left side surface, the bottom surface, and the top surface, whereby the expansion and contraction of the metal plate members due to temperature changes can be absorbed while airtightness is ensured.
The gas chromatograph apparatus according to the present invention includes the gas chromatograph column oven according to the present invention, a column accommodated in an internal space of the column oven, a sample introduction unit connected to an inlet end of the column, and a detection unit connected to an outlet end of the column.
Here, the detection method of the detection unit is not particularly limited, and various types of detection units used in gas chromatography apparatuses can be generally used. The sample introduction section is also similar to the above, and the sample introduction method is not limited to this, and the sample vaporized in the sample vaporization chamber may be introduced into the column, or the gaseous sample collected by the headspace method may be introduced into the column.
[ Effect of the invention ]
According to the column oven for gas chromatograph and the gas chromatograph apparatus using the same of the present invention, even when a combustible gas such as hydrogen gas accumulated in the internal space of the column oven chamber is ignited and explodes, the degree of the explosion can be reliably reduced as compared with the conventional apparatus. This can prevent, for example, a door from being opened suddenly, thereby preventing an accident such as a user being injured by the door hitting the user. Further, by reducing the degree of explosion, the degree of scattering of various members constituting the column oven, various members of the gas chromatograph apparatus main body in which the column oven is incorporated, and the like, toward the surroundings at the time of explosion can be suppressed.
Drawings
Fig. 1 is an external perspective view showing a state in which a door of a gas chromatograph main body incorporating a column oven for gas chromatograph according to an embodiment of the present invention is opened.
Fig. 2 is a perspective view of a column oven chamber main body of the column oven for gas chromatograph according to the present embodiment.
Fig. 3 is a perspective view of the column oven chamber main body of the column oven for gas chromatograph according to the present embodiment, as viewed from a direction different from that of fig. 2.
Fig. 4 is a diagram showing an assembly structure of a column oven chamber main body of the column oven for gas chromatograph according to the present embodiment.
Fig. 5 is a diagram illustrating a deformed state of the column oven chamber main body in the case where an explosion occurs in the internal space in the column oven for gas chromatograph according to the present embodiment.
FIG. 6 is a schematic configuration diagram of a gas chromatograph apparatus according to the present embodiment.
Fig. 7 is a schematic horizontal cross-sectional view (a) of a conventional column oven for a gas chromatograph with a door closed, and a partial substantially horizontal cross-sectional view (b) showing a state immediately after an explosion in an internal space.
Detailed Description
Next, an embodiment of a column oven for a gas chromatograph and a gas chromatograph apparatus using the same according to the present invention will be described with reference to the drawings.
FIG. 6 is a schematic configuration diagram of a gas chromatograph apparatus according to the present embodiment.
A column oven chamber main body 10 of a column oven for a gas chromatograph, which will be described later, is housed in a gas chromatograph apparatus main body 4, and a sample vaporizing chamber 1 and a detector 6 are attached to the gas chromatograph apparatus main body 4. A capillary column 5 is accommodated in an inner space 11 of the column incubator chamber main body 10, and an inlet end of the capillary column 5 is connected to the sample vaporizing chamber 1 and an outlet end thereof is connected to the detector 6. The detector 6 is not particularly limited in its form, and is, for example, a hydrogen Flame Ionization Detector (FID).
An appropriate carrier gas such as hydrogen gas or helium gas is supplied to the sample vaporization chamber 1 through the carrier gas flow path 2. When the sample vaporization chamber 1 is heated to an appropriate temperature and a small amount of the liquid sample is dropped from the syringe 3, the sample is vaporized in a short time and introduced into the capillary column 5 with the flow of the carrier gas. In the split injection method, most of the gas is discharged from the sample vaporization chamber 1 to the outside through a split flow path not shown, and only a part of the gas is introduced into the capillary column 5.
The column oven is controlled such that the temperature rises with the passage of time, for example, according to a predetermined temperature rise program, and while the sample gas passes through the capillary column 5, compounds in the sample gas are separated in the time direction and are sequentially introduced into the detector 6. The detector 6 generates a detection signal corresponding to the amount of the introduced compound, and inputs the detection signal to a signal processing unit, not shown. In the signal processing unit, a chromatogram is created from the obtained detection signal.
In this gas chromatograph apparatus, for example, when the connection between the capillary column 5 and the sample vaporizing chamber 1 is not proper, hydrogen gas used as a carrier gas accumulates in the internal space 11, and if the hydrogen gas is ignited by some factor, there is a possibility that explosion is caused. The column-temperature chamber main body 10 has a characteristic configuration so as to reduce the degree of such an explosion even when such an explosion occurs. Next, a characteristic configuration of the column oven main body 10 will be described.
Fig. 1 is an external perspective view showing a state in which a door of a gas chromatograph device main body 4 incorporating a column oven for gas chromatograph according to the present embodiment is opened, fig. 2 and 3 are perspective views of a column oven chamber main body 10, fig. 4 is a view showing an assembly structure of the column oven chamber main body 10, and fig. 5 is a view for explaining a state in which the column oven chamber main body 10 is deformed when an explosion occurs in an internal space 11. For convenience of explanation, in fig. 1 to 4, the width direction of the column oven chamber body 10 is defined as the X direction, the depth direction perpendicular to the X direction is defined as the Y direction, and the height direction perpendicular to both the X direction and the Y direction is defined as the Z direction.
As shown in fig. 1, the gas chromatograph apparatus main body 4 has a substantially rectangular parallelepiped housing 41, and an operation portion 42 provided with operation buttons and a display panel is provided on the right of the front surface of the housing 41. The column-temperature chamber main body 10 having an opening substantially over the entire front surface is housed in the case 41, and the front surface opening of the column-temperature chamber main body 10 is openable and closable by a door 12.
As shown in fig. 2, the column oven main body 10 is substantially rectangular parallelepiped in shape, and is composed of a right side wall portion 10a, a left side wall portion 10b, a top wall portion 10c, a bottom wall portion 10d, and a back wall portion 10 e. A frame-shaped front frame portion 10f is attached to the front edges of the right side wall portion 10a, the left side wall portion 10b, the top wall portion 10c, and the bottom wall portion 10d, and comes into close contact with the inner peripheral edge portion of the door 12 when the door 12 is closed. The five surfaces other than the front surface of the column oven main body 10, that is, the right side wall 10a, the left side wall 10b, the top wall 10c, the bottom wall 10d, and the back wall 10e, are all 3-layer structures having a heat insulating material such as glass wool interposed between the inner and outer 2 metal plates (in this example, the metal plate on the outer side of the bottom wall 10d substantially forms a part of the case 41).
As shown in fig. 4, the main members constituting the column oven main body 10 are an inner 1 st metal plate member 101 having a front view in a shape of substantially Contraband, an inner 2 nd metal plate member 102 having a side view in a shape of substantially inverted L, an outer 1 st metal plate member 103 having a top view in a shape of substantially Contraband, an outer metal foil member 104 which is a sheet material obtained by applying metal to an aluminum foil or a glass sheet, for example, which is not shown in fig. 4 but is seen in fig. 2, an outer 2 nd metal plate member 105 which is similarly not shown in fig. 4 but is seen in fig. 2, and a front frame metal plate member 106 having a substantially frame shape.
The inner 1 st metal plate member 101 is 1 metal plate member forming an inner wall of the right side wall portion 10a, the bottom wall portion 10d, and the left side wall portion 10 b. The inner 2 nd metal plate member 102 is 1 metal plate member forming an inner wall of the top wall portion 10c and the back wall portion 10 e. The outer 1 st metal plate member 103 is 1 metal plate member forming an outer wall of the right side wall portion 10a, the back wall portion 10e, and the left side wall portion 10 b. The outer metal foil member 104 is wound so as to cover the entire outer side of the heat insulating material in the bottom wall portion 10d, the top wall portion 10c, and the side wall portions 10a and 10b, and the outer 1 st metal plate member 103 is attached to the outer side of the outer metal foil member 104. Further, the outer 2 nd metal plate member 105 is a member mounted on the outer metal foil member 104 at the top face wall portion 10 c. In fig. 2 and 3, symbols indicating the respective components in fig. 4 are shown in parentheses ().
In the conventional column oven, the joint of the metal plate members is connected by welding to form the column oven chamber main body, particularly the inner wall surface facing the internal space 11. In contrast, in the column oven of the present embodiment, the joint between the inner 1 st metal plate member 101 and the inner 2 nd metal plate member 102, for example, the corner portions formed by the upper edge ends of the side wall portions 10a and 10b and the left and right edge ends of the top wall portion 10c coming into contact at substantially right angles are fixed to each other by fitting and screwing.
Specifically, as shown in fig. 4, the upper edge end of the portion of the inner 1 st metal plate member 101 corresponding to the both side wall portions 10a and 10b is bent inward at a substantially right angle to form an overlapping portion 1011, and an insertion opening 1012 elongated in the Y direction is formed at an appropriate portion of the bent portion. On the other hand, at both side edge ends of a portion of the inner 2 nd metal plate member 102 corresponding to the top wall portion 10c, protruding portions 1021 extending in tongue-like shapes toward both sides are formed at positions corresponding to the insertion ports 1012. By inserting the plurality of tab portions 1021 into the corresponding insertion ports 1012, the overlapping portions 1011 are brought into close contact with the portions of the inner 2 nd metal plate member 102 corresponding to the top wall portion 10c (the portions indicated by reference sign a in fig. 2).
As shown in fig. 3 and 4, an extension piece 1031 bent outward at a substantially right angle is formed at the upper edge of the outer 1 st metal plate member 103 at a portion corresponding to the both side wall portions 10a and 10 b. The extension piece 1031 is screwed to the outer 2 nd metal plate member 105.
Further, the front frame metal plate member 106 is also fixed to the outer 1 st metal plate member 103 by inserting and screwing the metal plate members. That is, as shown in fig. 2 to 4, both right and left sides of the substantially frame-shaped front frame metal plate member 106 are bent substantially at right angles to the rear side, and a plurality of tab portions 1062 extending in a tongue-like shape further rearward from the bent portion and having different extending lengths are formed. On the other hand, at the front edge of the portion of the outer 1 st metal plate member 103 corresponding to the side wall portions 10a and 10b, insertion ports 1032 elongated in the Z direction are formed at positions corresponding to the three central protruding portions 1062. The three projecting portions 1062 on the center side of the front frame metal plate member 106 are inserted into the insertion ports 1032 and fixed, and the two upper and lower projecting portions 1062 of the front frame metal plate member 106 are screwed to the outer 1 st metal plate member 103.
The front frame metal plate member 106, the inner 1 st metal plate member 101, and the inner 2 nd metal plate member 102 are not inserted or screwed, but are merely pressed and tightly bonded to each other so that no gap is formed in the joint therebetween. That is, the corner 1061 of the four corners inside the front frame metal plate member 106 has a substantially arc-like shape. The front frame metal plate member 106 is bent rearward at substantially right angles to the linear portions of the four inward sides to form overlapping portions 1063, and the corner portions 1061 at the four corners are also formed with extending portions 1064 extending rearward continuously to the overlapping portions 1063 at the two sides thereof. Such an extended portion 1064 bent at a substantially right angle at the corner of the curved shape can be formed satisfactorily by deep drawing by press working. When the front frame metal plate member 106 is fitted into the inner 1 st metal plate member 101 and the inner 2 nd metal plate member 102, the overlapping portion 1063 is pressed inward of the front edge portions of the inner 1 st metal plate member 10l and the inner 2 nd metal plate member 102, and a gap is hardly generated therebetween. Further, by forming the extended portion 1064 at the corner portion 1061 of the four corners, there is also an advantage as described later.
As shown in fig. 3 and 4, small holes 1033 are intermittently bored in the outer 1 st metal plate member 103 from the upper end and the lower end by a length of about 1/4 to 1/3 of the entire length at substantially right-angle bent portions between the portions corresponding to the side wall portions 10a and 10b and the portion corresponding to the rear wall portion 10e (see reference symbol D in fig. 3).
Further, circular or rectangular openings are formed in the inner 1 st metal plate member 101 at portions corresponding to the side wall portions 10a and 10b, and these openings are closed by the other metal plate member 107 from the side of the internal space 11.
In the gas chromatograph apparatus of the present embodiment using the column oven main body 10 having the above-described configuration, when hydrogen gas accumulates in the internal space 11 in which the door 12 is closed and is substantially sealed, and is ignited by heat, static electricity, or the like from the heater, explosion occurs. Then, the air pressure rises sharply in the internal space 11. As described above, the portion of the column oven main body 10 fixed by the insertion of the metal plate member is easily released when the air pressure in the internal space 11 is increased to a certain degree. Further, since the mechanical strength of the portion screwed by the narrow protruding piece portion 1021 is low, the internal space 11 is broken when the air pressure rises to some extent. In the portions where the small holes 1033 are intermittently formed, fine connection portions between the adjacent small holes 1033 are easily broken.
That is, in the column oven chamber main body 10, since the strength of the corner portion of the structure as described above is lower than the strength of the flat surface portion of the metal plate member, when the air pressure in the internal space 11 rises to a certain extent, the internal space is broken, or broken in advance, and an opening is formed. Once the opening is formed, the gas flows out of the opening at a stroke, and therefore, the metal plate member is deformed so that the opening is further enlarged. Specifically, as shown by the one-dot chain lines in fig. 5, the metal plate members are deformed to form a plurality of large openings, respectively. This opening functions as an explosion vent, and gas is discharged from the internal space 11 through this opening, whereby the increase in gas pressure in the internal space 11 is alleviated, and the scale of explosion is reduced. As a result, the extent to which various members constituting not only the column oven chamber main body 10 but also the gas chromatography apparatus main body 4 scatter around can be suppressed, and injury to personnel and loss of property can be reduced.
Further, as described above, in the column oven of the present embodiment, a large number of corners of the column oven chamber main body 10 are fixed by insertion or embedding of a metal plate. In such a portion, since there is a play between the metal plate members that are in contact with each other, even if the metal plate members expand and contract due to heat, a large load is not applied to the fixed portion. This can prevent the metal plate member from cracking.
In particular, in the temperature rise analysis, the metal plate member facing the internal space 11 reaches a high temperature of about 450 ℃ at the maximum, whereas the outer metal plate member only rises in temperature to about 150 ℃ at the maximum. Therefore, the temperature difference between the inner metal plate member and the outer metal plate member with the heat insulating material interposed therebetween may be extremely large. Since the front frame metal plate member 106 is in contact with both the inner metal plate member and the outer metal plate member, the difference in expansion and contraction due to temperature is large depending on the location. The stress caused by the expansion and contraction tends to concentrate on the corner 1061 of the four corners inside the front frame metal plate member 106, but in the column oven of the present embodiment, the corner 1061 has a substantially circular arc shape, and an extension 1064 bent at a substantially right angle is formed inside the corner. This makes it difficult for stress to concentrate on the corner 1061, thereby reducing the occurrence of cracks due to fatigue fracture.
In the column oven of the present embodiment, the column oven chamber body 10 can be assembled by a simple tool such as a screw driver without using welding. When a welding process is required in manufacturing, it is costly to prepare welding equipment at a final assembly site, and therefore, a member manufactured by welding in a factory is generally transported to the final assembly site and assembled. However, in this case, the outer dimensions of the members are large, and therefore the cost required for transportation is enormous.
In contrast, in the column oven of the present embodiment, the main member constituting the column oven chamber main body 10 is a flat plate-like, L-shaped, or Contraband-shaped metal plate member, and more than the box-like members can be transported with the same volume. This also has the advantage of reducing transportation costs.
The above-described embodiments are merely examples of the present invention, and it is needless to say that modifications, corrections, additions and the like are made as appropriate within the scope of the gist of the present invention and are included in the scope of the claims of the present application.
Description of the symbols
10-column incubator main body
10a right side wall part
10b left side wall part
10c ceiling wall part
10d bottom wall
10e rear wall
10f front frame part
101 inner side 1 st metal plate member
1011 overlapping part
1012 insertion opening
102 inner 2 nd metal plate member
1021 lug part
103 outer 1 st metal plate member
1031 extension piece
1032 insertion opening
1033 Small hole
104 outer side metal foil member
105 outer 2 nd metal plate member
106 front frame metal plate member
1061 corner
1062 Tab part
1063 overlap part
1064 extension
107 metal plate member
11 inner space
12 door
1 sample vaporizing chamber
2 carrier gas flow path
3 Syringe
4 gas chromatography device body
41 casing
42 operating part
5 capillary chromatographic column
6, a detector.

Claims (5)

1. A column oven for a gas chromatograph, comprising a column oven chamber main body having a substantially rectangular parallelepiped shape and an opening in a front surface, and a door for opening and closing the opening in the front surface of the column oven chamber main body, wherein an internal space for housing a chromatographic column is formed by the column oven chamber main body and the door,
the column-temperature chamber main body is formed by using at least 2 of metal plate members bent in a substantially Contraband shape or a substantially L shape or substantially flat plate-shaped metal plate members as wall surfaces of five surfaces of a right side surface, a left side surface, a bottom surface, a top surface and a back surface except a front surface,
at least one of the corners between the adjacent two surfaces formed by abutting the five different metal plate members, except the front surface, at right angles to each other, is a vent connection portion formed by connecting two metal plate members by fitting or screwing,
when the air pressure in the internal space rises to a predetermined level or more, the vent connection portion is detached, broken, or deformed in advance to form an opening functioning as an explosion vent,
in the column oven chamber main body, wall surfaces of five surfaces of a right side surface, a left side surface, a bottom surface, a top surface and a back surface are respectively of a 3-layer structure formed by sandwiching a heat insulating material between an inner metal plate and an outer metal plate, a metal plate member of a substantially frame shape is mounted on the metal plate member forming the right side surface, the left side surface, the bottom surface and the top surface in such a manner that end edges of the inner metal plate and the outer metal plate facing the front surface on the right side surface, the left side surface, the bottom surface and the top surface are blocked, corner portions between adjacent two surfaces formed by abutting the metal plate member of the substantially frame shape and the metal plate member forming the right side surface, the left side surface, the bottom surface and the top surface at a substantially right angle are used as connection portions for discharging, and the connection portions for discharging are formed by connecting the two metal plate members by a fitting or screwing method,
the metal plate member having a substantially frame shape is bent backward at substantially right angles toward the linear portions of the four inward sides, and the corner portion between any 2 adjacent linear portions has a substantially circular arc shape in front view.
2. The column oven for gas chromatograph of claim 1, wherein,
a perforated linear portion is provided at a bent portion of the metal plate member bent in a substantially Contraband-shape or a substantially L-shape, and small holes are intermittently formed along the bent position.
3. The column oven for gas chromatograph according to claim 2,
all of the corner portions between the adjacent two surfaces formed by abutting the five different metal plate members, which form the right side surface, the left side surface, the bottom surface, the top surface, and the back surface except the front surface, at substantially right angles to each other are defined as a drainage connecting portion formed by connecting two metal plate members by a fitting or screwing method.
4. The column oven for gas chromatograph according to claim 3,
at least a part of the connection portion for bleeding, which is formed by connecting two metal plate members by a fitting or screwing method, has a play between the two metal plate members.
5. A gas chromatography apparatus, characterized in that,
a column oven for gas chromatograph according to any one of claims 1 to 4, a column housed in an internal space of the column oven, a sample introduction section connected to an inlet end of the column, and a detection section connected to an outlet end of the column.
CN201710757198.1A 2017-05-12 2017-08-29 Column oven for gas chromatograph and gas chromatograph apparatus using the same Active CN108872456B (en)

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