CN108645943B - Fast heating gas chromatograph column box - Google Patents
Fast heating gas chromatograph column box Download PDFInfo
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- CN108645943B CN108645943B CN201810552666.6A CN201810552666A CN108645943B CN 108645943 B CN108645943 B CN 108645943B CN 201810552666 A CN201810552666 A CN 201810552666A CN 108645943 B CN108645943 B CN 108645943B
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- heating wire
- chromatographic column
- box body
- gas chromatograph
- spiral
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/60—Construction of the column
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/50—Conditioning of the sorbent material or stationary liquid
- G01N30/52—Physical parameters
- G01N30/54—Temperature
Abstract
The invention discloses a fast heating column box of a gas chromatograph, which relates to the technical field of gas chromatographs and has the technical scheme key points that: the chromatographic column comprises a box body and a chromatographic column arranged in the box body, wherein an inner heating wire and an outer heating wire are also arranged in the box body, the inner heating wire, the outer heating wire and the chromatographic column are all bent to be spiral, and the axes of the spiral formed by the inner heating wire, the outer heating wire and the chromatographic column are all coaxial; the chromatographic column is positioned in a spiral cavity formed by the external heating wire, and an external gap is reserved between the external heating wire and the chromatographic column; the inner heating wire is positioned in a spiral cavity formed by the chromatographic column, an inner gap is reserved between the inner heating wire and the chromatographic column, and the outer heating wire and the inner heating wire are electrically connected with a power supply. The gas chromatograph can measure the benzene series in the air, the chromatographic column of the column box is heated quickly and uniformly, and the detection can be started without waiting for a long time even if the equipment is in a cold state; and the temperature of the chromatographic column can be accurately regulated and controlled.
Description
Technical Field
The invention relates to the technical field of gas chromatographs, in particular to a rapidly-heated gas chromatograph column box.
Background
The gas chromatograph is an instrument for measuring components in a mixture, during measurement, an analysis sample is gasified in an injection port and then is carried into a chromatographic column by carrier gas, and according to the characteristic that each component in the mixture has different retention performances, each component is separated and is sequentially led into a detector to obtain a detection signal of each component. The components can be distinguished according to the sequence of leading in the detector and through comparison, the content of each component can be calculated according to the peak height or peak area, and the detector usually adopted is a thermal conductivity detector, a flame ionization detector and the like. In order to pass the sample gas through the column at a predetermined temperature, the column is generally heated by a column box, and the column is accommodated in the column box to adjust the temperature of the column.
Chinese patent application with prior application publication No. CN103293254A discloses a gas chromatography apparatus, which comprises a column-type heating furnace, a sample vaporizing chamber, a carrier gas supply unit, a detector, a control unit, and a hydrogen detection sensor, wherein a chromatographic column, a heater, and a radial fan are disposed in the column-type heating furnace.
Column type heating furnace is the post case, but the heater of current post case is inclined to one side in the incasement one end, and needs the fan to stir even to incasement heat, and rate of heating is slower, needs wait for longer time and just can detect when equipment is in the cold state.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a fast-heating gas chromatograph column box which has the advantage of high heating speed.
The technical purpose of the invention is realized by the following technical scheme: a fast heating gas chromatograph column box comprises a box body and a chromatographic column arranged in the box body, wherein an inner heating wire and an outer heating wire are further arranged in the box body, the inner heating wire, the outer heating wire and the chromatographic column are all bent to be spiral, and the axes of the spiral formed by the inner heating wire, the outer heating wire and the chromatographic column are all coaxial; the chromatographic column is positioned in a spiral cavity formed by the external heating wire, and an external gap is reserved between the external heating wire and the chromatographic column; the inner heating wire is positioned in a spiral cavity formed by the chromatographic column, an inner gap is reserved between the inner heating wire and the chromatographic column, and the outer heating wire and the inner heating wire are electrically connected with a power supply.
By the technical scheme, when heating is carried out, a sample is injected into one end of the chromatographic column, and the power supplies of the inner heating wire and the outer heating wire are started simultaneously; because the inner heating wire and the outer heating wire are respectively close to the chromatographic column and the heating area is spirally increased, the chromatographic column is heated quickly and uniformly without an additional fan for stirring the air in the box body; even when the device is in a cold state, the detection can be started without waiting for a long time.
Preferably, a heating gap is reserved between the spiral lines formed by the chromatographic column, and the spiral line formed by the outer heating wire is over against the heating gap.
Through above-mentioned technical scheme, when outer heater wire generates heat, the heat radiation of outer heater wire can direct action on the adjacent pipeline of chromatographic column, and the temperature of chromatographic column promotes very fast and is heated evenly.
Preferably, an outer separation frame is arranged in the outer gap, and separates the outer heating wire from the chromatographic column; an inner separation frame is arranged in the inner gap and separates the chromatographic column from the inner heating wire.
Through above-mentioned technical scheme, outer heater strip and chromatographic column are separated to outer partition frame, and inner partition frame separates interior heater strip and chromatographic column, avoids the three to take place direct contact and leads to the local high temperature of chromatographic column.
Preferably, the outer heating wire and the inner heating wire are independently heated by two power supplies respectively, and the two power supplies can independently adjust the voltage output to the outer heating wire or the inner heating wire.
Through the technical scheme, because the two power supplies for heating the inner heating wire and the outer heating wire can independently adjust the voltage output to the outer heating wire or the inner heating wire, the temperature of the outer heating wire and the temperature of the inner heating wire can be independently adjusted, and therefore the temperature of the chromatographic column can be accurately controlled.
Preferably, an outer temperature sensor is fixed on the outer heating wire, an inner temperature sensor is fixed on the inner heating wire, and an intermediate temperature sensor is fixed on the chromatographic column; and the box body is provided with a display device for displaying the temperature detected by the outer temperature sensor, the middle temperature sensor and the inner temperature sensor.
Through above-mentioned technical scheme, the temperature that three temperature sensor that shows through display device detected, relevant personnel can understand the temperature of interior heater strip, outer heater strip and chromatographic column directly perceivedly, is convenient for to the control of chromatographic column temperature.
Preferably, the inner wall of the box body is provided with a heat insulation layer.
Through above-mentioned technical scheme, the insulating layer is used for reducing the inside and outside heat exchange of box, reduces the energy loss.
Preferably, the inner heating wire can slide along the axial direction of the spiral of the inner heating wire, and a driving mechanism for driving the inner heating wire to slide is arranged on the box body.
Through the technical scheme, the driving mechanism drives the inner heating wire to move, so that the length of the inner heating wire in the spiral cavity of the chromatographic column is changed. When a sample in the chromatographic column just enters the box body, the sample is heated by the outer heating wire firstly, and when the sample reaches between the outer heating wire and the inner heating wire, the sample is heated by the two heating wires together. The temperature gradient is formed by the heating temperature for heating the samples which are too sensitive to the temperature change, the temperature of the samples is gradually increased, the samples are not easy to change in quality, and the application range of the gas chromatograph is enlarged.
Preferably, the driving mechanism comprises an adjusting rod rotatably arranged in the box body, the adjusting rod is in threaded connection with the box body, and the end part of the adjusting rod penetrates through the box body and is provided with a hand wheel; the adjusting rod is coaxial with the spiral axis of the inner heating wire, the inner heating wire is fixedly provided with the mounting frame, the adjusting rod is provided with a rotating groove matched with the mounting frame, and the inner heating wire can rotate relative to the adjusting rod and cannot axially move relative to the adjusting rod.
Through the technical scheme, under the normal condition, the inner heating wire is positioned at the mounting position under the supporting action of the mounting frame and the adjusting rod; when the hand wheel is rotated, the hand wheel drives the adjusting rod to rotate, the adjusting rod generates axial movement under the effect of threaded connection with the box body, and the adjusting rod drives the inner heating wire to move through the mounting frame.
Preferably, the adjusting rod is coaxially fixed with a driving gear, the box body is provided with a rack in a sliding manner, the rack is driven by the driving gear to slide, and the rack is provided with a pointer.
Through the technical scheme, when the adjusting rod rotates, the adjusting rod drives the inner heating wire to move and simultaneously drives the rack to slide through the driving gear, so that the position of the pointer is changed. Because the position of the pointer and the position of the inner heating wire are in a linear relation, a user can conveniently deduce the relative position between the inner heating wire and the chromatographic column through the position of the pointer, and the control of the heating temperature gradient is convenient.
In summary, compared with the prior art, the beneficial effects of the invention are as follows:
1. the chromatographic column is heated quickly and uniformly without a fan;
2. the over-high local temperature of the chromatographic column is prevented by arranging the inner separation frame and the outer separation frame;
3. the temperature of the chromatographic column can be accurately regulated and controlled, and the temperatures of the external heating wire, the internal heating wire and the chromatographic column can be displayed;
4. by arranging the driving mechanism, the heating temperature can form two gradients.
Drawings
Fig. 1 is a perspective view of a rapidly heated gas chromatograph column housing of an embodiment, mainly highlighting the external structure of the column housing;
FIG. 2 is a sectional view A-A of FIG. 1, mainly highlighting the internal structure of the spar-box;
fig. 3 is an exploded view of the interior of the column box, mainly highlighting the structure of the external shelf and the mounting rack.
Reference numerals: 1. a box body; 2. a chromatographic column; 3. an inner heating wire; 4. an outer heating wire; 11. a thermal insulation layer; 21. an interface; 41. an outer gap; 411. an outer spacer; 22. heating the gap; 31. an inner gap; 311. an inner partition frame; 5. adjusting a rod; 51. a hand wheel; 52. a driving gear; 53. a mounting frame; 531. mounting holes; 54. rotating the groove; 61. an external temperature sensor; 62. a medium temperature sensor; 63. an internal temperature sensor; 6. a display device; 71. a driven gear; 72. a rack; 721. a pointer.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
The present embodiment is only for explaining the present invention, and it is not limited to the present invention, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present invention.
As shown in fig. 1 and 2, a rapid heating column box of a gas chromatograph comprises a box body 1 and a chromatographic column 2 arranged in the box body 1, wherein an inner heating wire 3 and an outer heating wire 4 are further arranged in the box body 1, and the inner heating wire 3, the outer heating wire 4 and the chromatographic column 2 are all bent to be spiral and the formed spiral axes are all coaxial.
The box body 1 is cuboid, a box door for opening and closing is arranged on the box body 1, a heat insulation layer 11 made of asbestos is attached to the inner wall of the box body 1, and the heat insulation layer 11 is used for reducing heat exchange inside and outside the box body 1. The two ends of the chromatographic column 2 extend upwards to the inner top of the box body 1, the outer top of the box body 1 is provided with interfaces 21 which are respectively communicated with the two ends of the chromatographic column 2, and the two interfaces 21 are used for respectively inputting and outputting samples.
As shown in fig. 2 and 3, the diameters of the spirals formed by the external heating wire 4, the chromatographic column 2 and the internal heating wire 3 are sequentially reduced, the chromatographic column 2 is located in the spiral cavity formed by the external heating wire 4, and an external gap 41 is left between the external heating wire 4 and the chromatographic column 2. An outer separation frame 411 is arranged in the outer gap 41, the outer separation frame 411 is made of high-temperature-resistant resin, the outer heating wire 4 and the chromatographic column 2 are separated by the outer separation frame 411, and the phenomenon that the local temperature of the chromatographic column 2 is too high due to direct contact of the outer heating wire and the chromatographic column is avoided. Heating gaps 22 are reserved among the spiral lines formed by the chromatographic columns 2, and the spiral lines formed by the outer heating wires 4 are over against the heating gaps 22. The outer heating wire 4 is made of a copper pipe with a resistance wire in a penetrating mode, two ends of the outer heating wire are fixedly connected with the inner wall of the box body 1, and the outer heating wire 4 is powered by an independent power supply to generate heat. When the outer heating wire 4 generates heat, the heat radiation energy of the outer heating wire 4 directly acts on the adjacent pipeline of the chromatographic column 2, and the temperature of the chromatographic column 2 is increased quickly.
The inner heating wire 3 is positioned in a spiral cavity formed by the chromatographic column 2, and an inner gap 31 is reserved between the inner heating wire 3 and the chromatographic column 2. An inner separation frame 311 is arranged in the inner gap 31, the inner separation frame 311 is also made of high-temperature-resistant resin, the inner separation frame 311 is fixed with the chromatographic column 2 through static friction, the inner separation frame 311 separates the inner heating wire 3 from the chromatographic column 2, and the phenomenon that the local temperature of the chromatographic column 2 is too high due to direct contact of the inner heating wire and the chromatographic column is avoided. The inner heating wire 3 is also made of a copper pipe with a resistance wire in a penetrating way, the inner heating wire 3 can slide along the axis direction of the spiral of the inner heating wire, and the box body 1 is provided with a driving mechanism for driving the inner heating wire 3 to slide.
As shown in fig. 1 and 2, the driving mechanism comprises an adjusting rod 5 rotatably arranged in the box body 1, the adjusting rod 5 is coaxial with the spiral axis of the inner heating wire 3, one end of the adjusting rod 5 is in threaded connection with the box body 1 and penetrates out of the box body 1, and a hand wheel 51 is fixed at the end part of the adjusting rod; the other end of the adjusting rod 5 also penetrates through the box body 1, and the end part of the adjusting rod is coaxially fixed with a driving gear 52. The mounting frame 53 is fixed on the inner heating wire 3, the mounting hole 531 is formed in the center of the mounting frame 53, the annular rotary groove 54 is formed in the outer side wall of the adjusting rod 5, the mounting frame 53 is sleeved on the rotary groove 54 through the mounting hole 531, the inner heating wire 3 can rotate relative to the adjusting rod 5, and axial movement cannot be generated relative to the adjusting rod 5.
Under normal conditions, the inner heating wire 3 is in the installation position under the supporting action of the mounting frame 53 and the adjusting rod 5. When the hand wheel 51 is rotated, the hand wheel 51 drives the adjusting rod 5 to rotate, and the adjusting rod 5 generates axial movement under the effect of threaded connection with the box body 1, so that the length of the inner heating wire 3 in the spiral cavity of the chromatographic column 2 is changed. When a sample in the chromatographic column 2 just enters the box body 1, the sample is firstly heated by the outer heating wire 4, and when the sample reaches between the outer heating wire 4 and the inner heating wire 3, the sample is heated by the two heating wires together. The temperature gradient is formed by the heating temperature for heating the samples which are too sensitive to the temperature change, the temperature of the samples is gradually increased, the samples are not easy to change in quality, and the application range of the gas chromatograph is enlarged.
The two ends of the inner heating wire 3 are electrically connected with an independent power supply through leads. The two power supplies for heating the inner heating wire 3 and the outer heating wire 4 can independently adjust the voltage output to the outer heating wire 4 or the inner heating wire 3, and then the temperatures of the outer heating wire 4 and the inner heating wire 3 can be independently adjusted, so that the temperature of the chromatographic column 2 can be accurately controlled.
As shown in fig. 1 and 3, an outer temperature sensor 61 is fixed on the outer heating wire 4, an inner temperature sensor 63 is fixed on the inner heating wire 3, and an intermediate temperature sensor 62 is fixed on the chromatographic column 2; the outer top wall of the box body 1 is provided with a display device 6 for displaying the temperatures detected by the outer temperature sensor 61, the middle temperature sensor 62 and the inner temperature sensor 63. Through the temperature that three temperature sensor that display device 6 shows detected, relevant personnel can know the temperature of interior heater strip 3, outer heater strip 4 and chromatographic column 2 directly perceivedly, be convenient for to the control of chromatographic column 2 temperature.
The casing 1 is provided with a driven gear 71 rotatably disposed on a side wall of the driving gear 52, the driven gear 71 is engaged with the driving gear 52, wherein the driving gear 52 has a thickness larger than that of the driven gear 71, and when the driving gear 52 moves along an axial direction thereof, the two gears can still be engaged. A rack 72 engaged with the driven gear 71 is slidably provided on the case 1, and a pointer 721 is fixed to the rack 72. When the adjusting lever 5 rotates, the adjusting lever 5 drives the inner heating wire 3 to move, and the adjusting lever 5 drives the rack 72 to slide by the meshing action of the driving gear 52 and the driven gear 71, thereby changing the position of the pointer 721. Since the position of the pointer 721 and the position of the inner heating wire 3 are in a linear relationship, the user can easily deduce the relative position between the inner heating wire 3 and the chromatographic column 2 by the position of the pointer 721, which facilitates the control of the heating temperature gradient.
When heating is performed, a sample is injected into one end of the chromatographic column 2, and simultaneously, the power supply of the inner heating wire 3 and the outer heating wire 4 is started. Because the inner heating wire 3 and the outer heating wire 4 are respectively close to the chromatographic column 2 and the heating area is spirally increased, the chromatographic column 2 is heated quickly and uniformly without an additional fan for stirring the air in the box body 1; even when the device is in a cold state, the detection can be started without waiting for a long time.
The above description is intended to be illustrative of the present invention and not to limit the scope of the invention, which is defined by the claims appended hereto.
Claims (8)
1. The utility model provides a rapid heating's gas chromatograph column case, includes box (1), sets up chromatographic column (2) in box (1), characterized by: an inner heating wire (3) and an outer heating wire (4) are further arranged in the box body (1), the inner heating wire (3), the outer heating wire (4) and the chromatographic column (2) are all bent to be spiral, and the axes of the spiral formed by the inner heating wire (3), the outer heating wire (4) and the chromatographic column (2) are all coaxial; the chromatographic column (2) is positioned in a spiral cavity formed by the external heating wire (4), and an external gap (41) is reserved between the external heating wire (4) and the chromatographic column (2); the inner heating wire (3) is positioned in a spiral cavity formed by the chromatographic column (2), an inner gap (31) is reserved between the inner heating wire (3) and the chromatographic column (2), and the outer heating wire (4) and the inner heating wire (3) are electrically connected with a power supply;
the inner heating wire (3) can slide along the spiral axis direction, and a driving mechanism for driving the inner heating wire (3) to slide is arranged on the box body (1).
2. The rapidly heated gas chromatograph column housing of claim 1, wherein: a heating gap (22) is reserved between the spiral lines formed by the chromatographic column (2), and the spiral lines formed by the outer heating wires (4) are opposite to the heating gap (22).
3. The rapidly heated gas chromatograph column housing of claim 1, wherein: an outer separation frame (411) is arranged in the outer gap (41), and the outer separation frame (411) separates the outer heating wire (4) from the chromatographic column (2); an inner separation frame (311) is arranged in the inner gap (31), and the chromatographic column (2) and the inner heating wire (3) are separated by the inner separation frame (311).
4. The rapidly heated gas chromatograph column housing of claim 1, wherein: the outer heating wire (4) and the inner heating wire (3) are independently heated by two power supplies respectively, and the two power supplies can independently adjust the voltage output to the outer heating wire (4) or the inner heating wire (3).
5. The rapidly heated gas chromatograph column housing of claim 4, wherein: an outer temperature sensor (61) is fixed on the outer heating wire (4), an inner temperature sensor (63) is fixed on the inner heating wire (3), and an intermediate temperature sensor (62) is fixed on the chromatographic column (2); the box body (1) is provided with a display device (6) for displaying the temperatures detected by the outer temperature sensor (61), the middle temperature sensor (62) and the inner temperature sensor (63).
6. The rapidly heated gas chromatograph column housing of claim 1, wherein: the inner wall of the box body (1) is provided with a heat insulation layer (11).
7. The rapidly heated gas chromatograph column housing of claim 1, wherein: the driving mechanism comprises an adjusting rod (5) which is rotatably arranged in the box body (1), the adjusting rod (5) is in threaded connection with the box body (1), and the end part of the adjusting rod (5) penetrates through the box body (1) and is provided with a hand wheel (51); the spiral axis of adjusting pole (5) and interior heater strip (3) is coaxial, be fixed with mounting bracket (53) on interior heater strip (3), set up on adjusting pole (5) with mounting bracket (53) complex rotary trough (54), interior heater strip (3) can rotate for adjusting pole (5), and can't produce axial displacement for adjusting pole (5).
8. The rapidly heated gas chromatograph column housing of claim 7, wherein: the adjusting rod (5) is coaxially fixed with a driving gear (52), a rack (72) is arranged on the box body (1) in a sliding mode, the rack (72) is driven by the driving gear (52) to slide, and a pointer (721) is arranged on the rack (72).
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810552666.6A CN108645943B (en) | 2018-05-31 | 2018-05-31 | Fast heating gas chromatograph column box |
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| CN201810552666.6A CN108645943B (en) | 2018-05-31 | 2018-05-31 | Fast heating gas chromatograph column box |
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| CN108645943B true CN108645943B (en) | 2020-05-05 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SG11201803540YA (en) | 2015-10-30 | 2018-05-30 | Torion Technologies Inc | Thermal gradient chromatography devices and methods of using them |
| CN109709247A (en) * | 2019-02-27 | 2019-05-03 | 辽东学院 | A kind of gas chromatograph post case quickly heated |
| CN110596289B (en) * | 2019-10-17 | 2024-03-22 | 钢研纳克检测技术股份有限公司 | Chromatographic column device capable of rapidly increasing and decreasing temperature |
| CN111796045B (en) * | 2020-07-13 | 2022-06-14 | 杭州道宇检测技术有限公司 | Chromatographic column heating device for gas chromatograph |
| CN112034081B (en) * | 2020-09-07 | 2022-12-13 | 浙江安联检测技术服务有限公司 | High-efficient heating gas chromatography device |
| CN112540140B (en) * | 2020-12-16 | 2022-12-27 | 中船(邯郸)派瑞特种气体股份有限公司 | Equipment and method for measuring trace impurities in HF (hydrogen fluoride) by gas chromatography |
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| EP2421624B1 (en) * | 2009-04-22 | 2013-06-12 | Karlsruher Institut für Technologie | Method and device for the sorptive separation of substance mixtures |
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