CN115308324A - Transmission line and device for combined use of gas chromatograph and mass spectrometer, temperature control transmission line and method - Google Patents

Transmission line and device for combined use of gas chromatograph and mass spectrometer, temperature control transmission line and method Download PDF

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Publication number
CN115308324A
CN115308324A CN202210900178.6A CN202210900178A CN115308324A CN 115308324 A CN115308324 A CN 115308324A CN 202210900178 A CN202210900178 A CN 202210900178A CN 115308324 A CN115308324 A CN 115308324A
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transmission line
mass spectrometer
capillary
gas chromatograph
temperature
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CN202210900178.6A
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Chinese (zh)
Inventor
杨记龙
徐振
李书阳
程文播
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Tianjin Guoke Medical Technology Development Co ltd
Suzhou Institute of Biomedical Engineering and Technology of CAS
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Tianjin Guoke Medical Technology Development Co Ltd
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Priority to CN202210900178.6A priority Critical patent/CN115308324A/en
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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
    • 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
    • G01N30/62Detectors specially adapted therefor
    • G01N30/72Mass spectrometers
    • G01N30/7206Mass spectrometers interfaced to gas chromatograph
    • 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
    • G01N30/88Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
    • 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
    • G01N2030/3084Control of physical parameters of the fluid carrier of temperature ovens

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

The invention relates to a transmission line, a device, a temperature control transmission line and a method for the combination of a gas chromatograph and a mass spectrometer, wherein the transmission line comprises: adapter, capillary protection tube, capillary, mounting, a plurality of heating element, lagging casing, capillary sealing joint, the one end of capillary protection tube is passed through the adapter and is installed on the mass spectrometer ionization chamber lateral wall of mass spectrometer detector cavity, the capillary protection tube cover is outside the capillary, the other end of capillary protection tube passes through capillary sealing joint with the capillary and fixes, heating element passes through the mounting to be fixed on the capillary protection tube, lagging casing installs outside the mounting. Because the transmission line has simple structure, easy processing and convenient maintenance, the air tightness of the chromaticness combination system and the reliability of the product are easier to be ensured, and the transmission line has excellent transmission effect.

Description

Transmission line and device for combined use of gas chromatograph and mass spectrometer, temperature control transmission line and method
Technical Field
The invention relates to the technical field of instruments and meters, in particular to a gas chromatograph and mass spectrometer combined transmission line, a device, a temperature control transmission line and a method.
Background
Mass Spectrometry (MS) is a spectroscopic method for determining the composition of compounds of ions by measuring the exact mass of the ions after separation of the moving ions by their mass-to-charge ratio using electric and/or magnetic fields, and is mainly used for structural identification of compounds, for example: molecular weight, elemental composition, and functional groups of the compound. Mass spectrometers for mass spectrometry are generally effective only for the detection of pure substances. In general, each component of the mixture is separated and then detected separately by a mass spectrometer.
Gas chromatography (abbreviated as GC) is a widely used separation means. It is a column chromatography with an inert gas as the mobile phase based on the difference in the distribution of the components in the sample between the two phases. Gas chromatography, while it can separate the individual components of a complex mixture, has poor qualitative ability.
At present, gas chromatography-mass spectrometry (GC-MS) is mainly used for separating and detecting complex mixtures. Gas chromatography and mass spectrometry are complementary in nature, and their combination provides a powerful tool for many analytical applications requiring high sensitivity and accuracy. However, these two instruments operate in very different environments, and therefore require a special connection device to couple the two instruments. The main difficulty of GC-MC is the difference between the two working pressures, the outlet pressure of the gas chromatographic column is generally atmospheric pressure, and the mass spectrometer works in a high vacuum environment (generally lower than 10^ -3 Pa). As mass spectrometers and gas chromatographs have evolved, temperature fluctuations (particularly cold spots) during effluent transport can lead to condensation from the gas phase and/or excessive peak broadening, making the transport lines for conventional chromatograph-mass spectrometers structurally unsatisfactory.
Disclosure of Invention
To achieve the above objects and other advantages and in accordance with the purpose of the invention, a first object of the present invention is to provide a combined transmission line of a gas chromatograph and a mass spectrometer, comprising: adapter, capillary protection tube, capillary, mounting, a plurality of heating element, lagging casing, capillary sealing joint, the one end of capillary protection tube is passed through the adapter is installed on the mass spectrometer ionization chamber lateral wall of mass spectrometer detector cavity, capillary protection tube sleeve is in outside the capillary, the other end of capillary protection tube with the capillary passes through capillary sealing joint fixedly, heating element passes through the mounting is fixed on the capillary protection tube, lagging casing installs outside the mounting.
Further, still include temperature sensor, temperature sensor passes through the mounting is fixed on the capillary protection tube.
Furthermore, the fixing part is a ceramic rod, a through hole in clearance fit with the outer diameter of the capillary tube protection tube is formed in the ceramic rod, a plurality of first blind holes are formed in the ceramic rod, the heating element is installed in the first blind holes, second blind holes are formed in the ceramic rod, and the temperature sensor is installed in the second blind holes.
Further, the lagging casing includes first lagging casing and second lagging casing, first lagging casing with the second lagging casing is arranged in outside the ceramic rod, first lagging casing with the second lagging casing is fixed on the mass spectrometer ionization chamber lateral wall of mass spectrometer detector cavity, the power cord mounting hole has been seted up on the second lagging casing, the power cord mounting hole is used for wearing out heating element's power cord reaches temperature sensor's control line.
Further, the adapter is an adapter with a sealing ring;
still include O type sealing washer, O type sealing washer is arranged in the slot of adapter and mass spectrometer ionization chamber lateral wall installation department.
Further, the ceramic rod connector also comprises an asbestos heat insulation pad which is arranged between the adapter and the ceramic rod;
gaps among the first heat-preservation shell, the second heat-preservation shell and the ceramic rod are filled with high-temperature-resistant heat-insulating materials;
the first blind holes are uniformly formed in the circumferential direction of the ceramic rod.
A second object of the present invention is to provide a combined gas chromatograph and mass spectrometer apparatus, comprising: microcontroller, input device, communication module, D/A converter, electric heat executor, A/D converter, the input device the communication module the D/A converter, the A/D converter with microcontroller connects, the D/A converter with the electric heat executor is connected, the electric heat executor with the heating element of gas chromatograph and mass spectrometer antithetical couplet transmission line be connected, the A/D converter with the temperature sensor of gas chromatograph and mass spectrometer antithetical couplet transmission line is connected.
Further, the electrothermal actuator comprises an inverter and a solid-state relay, the microcontroller is connected with the inverter through the D/A converter, the inverter is connected with the solid-state relay, and the solid-state relay is connected with the heating element;
the intelligent alarm system is characterized by further comprising a display and an alarm device, wherein the display and the alarm device are connected with the microcontroller.
The third purpose of the invention is to provide a temperature control transmission line for the combination of the gas chromatograph and the mass spectrometer, which comprises the transmission line for the combination of the gas chromatograph and the mass spectrometer and the device for the combination of the gas chromatograph and the mass spectrometer.
The fourth purpose of the invention is to provide a temperature control method of a temperature control transmission line for the combination of a gas chromatograph and a mass spectrometer, which comprises the following steps:
calculating the temperature difference between the set transmission line temperature and the acquired current transmission line temperature;
calculating a duty ratio according to the calculated temperature difference;
controlling the heating rate of the heating element according to the calculated duty ratio, and controlling the heating element to heat at a first heating rate when the acquired current temperature of the transmission line is lower than a temperature threshold value; when the acquired current temperature of the transmission line is not lower than the temperature threshold value, controlling the heating element to heat at a second heating rate; wherein the first heating rate is greater than the second heating rate.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a transmission line for the combination of a gas chromatograph and a mass spectrometer. A capillary tube with the inner diameter of 0.25-0.32mm widely adopted in GC-MC analysis is used as an introduction interface, the tail end of a capillary chromatographic column is directly inserted into an ion source of a mass spectrometer, and a carrier gas flows out of the gas chromatographic column together with components under the condition of a certain flow rate of the carrier gas and directly enters an action field of the ion source. The carrier gas is not ionized, the component to be detected forms charged ions, the charged ions are accelerated to move to the mass analyzer under the action of the accelerating electric field, and the carrier gas can be pumped away by the vacuum pump maintaining negative pressure. Since the carrier gas flow rate is limited by the vacuum pump flow rate in the mass spectrometer, the carrier gas flow rate should be controlled to be around 50% of the maximum flow rate of the vacuum pump. The maximum working temperature of the interface is close to the maximum column temperature of the chromatograph. The interface device has simple structure and easy maintenance, and the sample transmission rate reaches 100 percent.
The gas chromatograph and the mass spectrometer connected by the transmission line have the advantages that the transmission line is simple in structure, easy to process and convenient to maintain, so that the air tightness of a chromaticness and mass spectrometer system and the reliability of a product are ensured more easily, and the transmission effect is excellent. In addition, the size of the transmission line can be adjusted adaptively according to the requirements of interfaces of a gas chromatograph and a mass spectrometer, so that the transmission line can meet the requirements of miniaturization and intellectualization of the structure, and can be designed in series according to the requirements, meet the requirements of rapid design and meet the requirements of the market as soon as possible.
The heating holes are uniformly arranged on the ceramic rod so as to uniformly heat the gas in the transmission line main body. And the temperature measuring holes are arranged on the symmetrical surface of the heating rod, so that the uniformity of temperature is improved, and the heating efficiency is improved. A ceramic material with good thermal conductivity, such as alumina ceramic, is used so that the heat distribution along the transmission line is homogeneous and constant.
And heating and temperature monitoring of the gas in the capillary are realized by adopting a heating element and a temperature sensor. The temperature sensor also plays a role in limiting the heating element while realizing temperature sensing.
A variable rate temperature control algorithm is employed so that during operation there are no cold spots that can cause condensation of the analyte and hence peak broadening and hot spots that can cause decomposition of the analyzed compound.
The highest working temperature of the transmission line is close to the highest column temperature, the authenticity of detection is guaranteed, the interface is simple, the maintenance is easy, and the transmission efficiency is extremely high and close to 100%.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to implement them in accordance with the contents of the description, the following detailed description is given with reference to the preferred embodiments of the present invention and the accompanying drawings. The detailed description of the present invention is given in detail by the following examples and the accompanying drawings.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the invention without limiting the invention. In the drawings:
FIG. 1 is a schematic diagram of the connection of a transmission line of example 1 with a gas chromatograph and a mass spectrometer;
FIG. 2 is a first side view of the transmission line shaft of embodiment 1;
FIG. 3 is a second side view of the transfer spool of embodiment 1;
FIG. 4 is a first perspective view of a transmission line segment part of example 1;
FIG. 5 is a second perspective view of a transmission line section of example 1;
FIG. 6 is a schematic view of a combination of a gas chromatograph and a mass spectrometer according to example 2;
FIG. 7 is a schematic view of an electrothermal actuator according to embodiment 2;
FIG. 8 is a schematic view of the on-off control of the heating element;
FIG. 9 is a graph of temperature difference t as a function of duty cycle φ;
FIG. 10 is a flowchart of a temperature control method of the gas chromatograph and mass spectrometer combination temperature controlled transmission line of example 4.
In the figure: 1. a transmission line; 11. a first heat-insulating housing; 12. a second insulated housing; 121. a power line mounting hole; 13. a ceramic rod; 14. a capillary tube protection tube; 15. a capillary seal joint; 16. a capillary tube; 17. an adapter; 18. an asbestos insulation mat; 19. a heating element; 110. a temperature sensor; 2. a mass spectrometer detector cavity; 21. a side wall of the ionization chamber of the mass spectrometer; 3. a cavity of a gas chromatograph.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and the detailed description, and it should be noted that any combination of the embodiments or technical features described below can be used to form a new embodiment without conflict.
Example 1
A combined gas chromatograph and mass spectrometer transmission line 1, as shown in fig. 1 to 5, comprising: adapter 17, capillary protection tube 14, capillary 16, the mounting, a plurality of heating element 19, the heat preservation shell, capillary sealing joint 15, the one end of capillary protection tube 14 is installed on the mass spectrometer ionization chamber lateral wall 21 of mass spectrometer detector cavity 2 through adapter 17, capillary protection tube 14 cover is outside capillary 16, the other end of capillary protection tube 14 is fixed through capillary sealing joint 15 with capillary 16, heating element 19 is fixed on capillary protection tube 14 through the mounting, the heat preservation shell is installed outside the mounting. In this embodiment, the heating element 19 is a heating resistor.
Transmission line main part one end is passed through flange and is connected with the mass spectrograph, and the other end is connected with gas chromatograph. The capillary 16 with the inner diameter of 0.25-0.32mm widely used in GC-MC analysis is used as an introduction interface, the tail end of a chromatographic column of the capillary 16 is directly inserted into an ion source of a mass spectrometer, and under the condition of a certain flow rate of carrier gas, the carrier gas carries components to flow out of the gas chromatographic column and directly enters an action field of the ion source. The carrier gas is not ionized, the component to be detected forms charged ions, the charged ions are accelerated to move to the mass analyzer under the action of the accelerating electric field, and the carrier gas can be pumped away by the vacuum pump maintaining negative pressure. Since the carrier gas flow rate is limited by the vacuum pump flow rate in the mass spectrometer, the carrier gas flow rate should be controlled to be around 50% of the maximum flow rate of the vacuum pump. The maximum working temperature of the interface is close to the maximum column temperature of the chromatograph. The interface device has simple structure and easy maintenance, and the sample transmission rate reaches 100 percent.
To ensure the tightness of the mass spectrometer detector cavity 2. Preferably, the adapter 17 is an adapter 17 with a sealing ring; one end of the adapter 17 with the sealing ring is screwed into a threaded hole of a sealing conical tube of the ionization chamber side wall 21 of the mass spectrometer, and an O-shaped sealing ring is added into a groove in the adapter for sealing, so that air leakage of a vacuum cavity of the ionization chamber is avoided.
The capillary tube protection tube 14 penetrates through the adapter 17 with the sealing ring, the conical gasket of the adapter 17 with the sealing ring is forced to deform by screwing down the adapter 17 with the sealing ring, so that the outer side of the capillary tube protection tube 14 is sealed, air leakage at the contact part of the adapter 17 with the sealing ring and the capillary tube protection tube 14 is avoided,
in order to monitor the temperature of the gas within the capillary tube 16. Further, a temperature sensor 110 is included, and the temperature sensor 110 is fixed on the capillary protection tube 14 by a fixing member. In this embodiment, the temperature sensor 110 is a PT100 temperature sensor.
The fixing member is a ceramic rod 13, and the ceramic rod 13 is provided with a through hole in clearance fit with the outer diameter of the capillary protection tube 14, for example, the through hole can be formed at the center of the ceramic rod 13, so that the capillary protection tube 14 passes through the ceramic rod 13. The ceramic rod 13 is provided with a plurality of first blind holes, and the heating element 19 is arranged in the first blind holes. Preferably, a plurality of first blind holes are uniformly arranged along the circumferential direction of the ceramic rod 13, and the heating element 19 is installed in the first blind holes in the circumferential direction of the ceramic rod 13, and is in clearance fit for installation, and the precision grade is determined to be 7. The ceramic rod 13 is provided with a second blind hole, and the temperature sensor 110 is installed in the second blind hole. Specifically, a second blind hole for installing the temperature sensor 110 is machined at the symmetrical center plane of the ceramic rod 13, and the temperature sensor 110 is installed in the blind hole at the position, and the blind hole is in clearance fit.
The heat preservation shell includes first heat preservation shell 11 and second heat preservation shell 12, first heat preservation shell 11 and second heat preservation shell 12 are the cotton shell that keeps warm, first heat preservation shell 11 and second heat preservation shell 12 are arranged in outside ceramic rod 13, first heat preservation shell 11 and second heat preservation shell 12 are fixed on mass spectrometer ionization chamber lateral wall 21 of mass spectrometer detector cavity 2, power cord mounting hole 121 has been seted up on second heat preservation shell 12, power cord mounting hole 121 is used for wearing out heating element 19's power cord and temperature sensor 110's control line. The power line of the heating element 19 and the control line of the temperature sensor 110 penetrate out of the power line mounting hole 121 on the second heat-insulating shell 12 on the basis of electromagnetic shielding, the first heat-insulating shell 11 and the second heat-insulating shell 12 are fixed on the ionization chamber side wall 21 of the mass spectrometer through bolts, and a gap position inside the first heat-insulating shell 11 and the second heat-insulating shell 12 is filled with high-temperature-resistant heat-insulating materials, such as glass fiber cotton, which play a role in heat insulation and prevent heat waste; meanwhile, the damage caused by the touch of a person on the first heat-preservation shell 11 and the second heat-preservation shell 12 is avoided, and the other end of the transmission line 1 extends into the cavity 3 of the gas chromatograph.
Further, an asbestos heat insulation pad 18 is further included, and the asbestos heat insulation pad 18 is installed between the adapter 17 and the ceramic rod 13. Specifically, the asbestos heat insulation pad 18 is mounted on one end of the adapter 17 with the sealing ring and is attached tightly, and the other surface of the asbestos heat insulation pad 18 is attached tightly to the end surface of the ceramic rod 13.
Example 2
A combination gas chromatograph and mass spectrometer apparatus, as shown in fig. 6, comprising: the system comprises a microcontroller, an input device, a communication module, a D/A converter, an electric heating actuator and an A/D converter, wherein the input device, the communication module, the D/A converter and the A/D converter are connected with the microcontroller, the D/A converter is connected with the electric heating actuator, the electric heating actuator is connected with a heating element 19 of a transmission line for the combination of a gas chromatograph and a mass spectrometer, and the A/D converter is connected with a temperature sensor 110 of the transmission line for the combination of the gas chromatograph and the mass spectrometer. In this embodiment, the input device is a keyboard, and is used to input the temperature to be set for the transmission line. The communication module is a USB/RS485 communication interface and is used for transmitting real-time data to the upper computer and displaying and controlling the temperature of the user interface. The device carries out negative feedback constant temperature control on the temperature by a temperature control method, and controls the fluctuation range of the temperature. For the detailed description of the method, reference may be made to the corresponding description in the following method embodiments, which are not repeated herein.
As shown in fig. 7, the electrothermal actuator includes an inverter and a solid-state relay, the microcontroller is connected to the inverter via a D/a converter, the inverter is connected to the solid-state relay, and the solid-state relay is connected to the heating element 19. Because the load capacity of the output end of the microcontroller is not strong, the load capacity of the output end of the microcontroller is improved through the phase inverter. The microcontroller controls the on-off of the strong power end of the solid-state relay by controlling the high and low levels of the output end. The solid relay separates the weak current of the control circuit from the strong current heated by the heating element 19, and can effectively protect the circuit and the lead, so that the strong current and the weak current do not interfere with each other, work respectively, and have better electrical insulation capability and interference prevention capability.
As shown in fig. 6, the device also comprises a display and an alarm device, wherein the display and the alarm device are connected with the microcontroller. In this embodiment, the display is an LED display for displaying the current temperature and the set temperature. And the alarm device is used for carrying out overtemperature alarm in the constant temperature control process, and preventing the transmission line from being burnt due to overhigh temperature caused by line faults.
Example 3
The third purpose of the invention is to provide a temperature-controlled transmission line for the combination of the gas chromatograph and the mass spectrometer, which comprises the transmission line for the combination of the gas chromatograph and the mass spectrometer of the embodiment 1 and the combination device for the gas chromatograph and the mass spectrometer of the embodiment 2. Reference may be made to the corresponding description in the above method embodiments, which is not repeated herein.
Example 4
The temperature control method of the combined temperature-controlled transmission line for the gas chromatograph and the mass spectrometer in the embodiment 3, as shown in fig. 10, includes the following steps:
calculating the temperature difference between the set transmission line temperature and the acquired current transmission line temperature; in particular, the amount of the solvent to be used,
t=t is provided with -t At present
Wherein t is the temperature difference, t Is provided with To setTemperature of transmission line, t At present The current temperature of the transmission line is collected.
As shown in FIG. 8, the control period of the heating element 19 is T, and the time period during which the heating element 19 is turned on is T on ,φ=T on /T,
Figure BDA0003770577700000081
As shown in fig. 9, the microcontroller calculates the duty ratio phi by the temperature difference t measured in real time, and then controls the heating rate of the heating element 19. So that when the temperature is low, such as when the current temperature of the transmission line being collected is below a temperature threshold, the heating element 19 is controlled to heat at a first heating rate so that the temperature can rise at a faster rate; when the temperature is close to the set temperature, for example, when the collected current temperature of the transmission line is not lower than the temperature threshold, the heating element 19 is controlled to heat at the second heating rate, so that the temperature rises at a lower rate, thermal shock is avoided, that is, thermal shock when the temperature reaches the set temperature is avoided, and the oscillation amplitude of the temperature curve is reduced.
It should also be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrases "comprising one of 8230; \8230;" 8230; "does not exclude the presence of additional like elements in a process, method, article, or apparatus that comprises the element.
The embodiments in the present specification are described in a progressive manner, and the same and similar parts among the embodiments are referred to each other, and each embodiment focuses on the differences from the other embodiments.
The foregoing is merely an example of the present specification and is not intended to limit one or more embodiments of the present specification. Various modifications and alterations to one or more embodiments described herein will be apparent to those skilled in the art. Any modification, equivalent replacement, improvement or the like made within the spirit and principle of one or more embodiments of the present disclosure should be included in the scope of claims of one or more embodiments of the present disclosure. One or more embodiments of this specification.

Claims (10)

1. A transmission line for combined use of a gas chromatograph and a mass spectrometer is characterized by comprising: adapter, capillary protection tube, capillary, mounting, a plurality of heating element, lagging casing, capillary sealing joint, the one end of capillary protection tube is passed through the adapter is installed on the mass spectrometer ionization chamber lateral wall of mass spectrometer detector cavity, capillary protection tube sleeve is in outside the capillary, the other end of capillary protection tube with the capillary passes through capillary sealing joint fixedly, heating element passes through the mounting is fixed on the capillary protection tube, lagging casing installs outside the mounting.
2. The combined transmission line for a gas chromatograph and a mass spectrometer of claim 1, wherein: still include temperature sensor, temperature sensor passes through the mounting is fixed on the capillary protection tube.
3. The combined transmission line for a gas chromatograph and a mass spectrometer of claim 2, wherein: the fixing piece is a ceramic rod, a through hole in clearance fit with the outer diameter of the capillary tube protection tube is formed in the ceramic rod, a plurality of first blind holes are formed in the ceramic rod, the heating element is installed in the first blind holes, second blind holes are formed in the ceramic rod, and the temperature sensor is installed in the second blind holes.
4. The transmission line for the combined use of a gas chromatograph and a mass spectrometer according to claim 3, characterized in that: the thermal insulation shell comprises a first thermal insulation shell and a second thermal insulation shell, the first thermal insulation shell and the second thermal insulation shell are arranged outside the ceramic rod, the first thermal insulation shell and the second thermal insulation shell are fixed on the side wall of a mass spectrometer ionization chamber of a mass spectrometer detector cavity, a power line mounting hole is formed in the second thermal insulation shell, and the power line mounting hole is used for penetrating out a power line of the heating element and a control line of the temperature sensor.
5. The transmission line for the combined use of a gas chromatograph and a mass spectrometer according to claim 1, characterized in that: the adapter is an adapter with a sealing ring;
still include O type sealing washer, the O type sealing washer is arranged in the slot of adapter and the installation of mass spectrograph ionization chamber lateral wall department.
6. The combined transmission line for a gas chromatograph and a mass spectrometer of claim 4, wherein: the ceramic rod is characterized by also comprising an asbestos heat insulation pad, wherein the asbestos heat insulation pad is arranged between the adapter and the ceramic rod;
gaps among the first heat-preservation shell, the second heat-preservation shell and the ceramic rod are filled with high-temperature-resistant heat-insulating materials;
and the plurality of first blind holes are uniformly arranged along the circumferential direction of the ceramic rod.
7. A combined gas chromatograph and mass spectrometer device, comprising: the system comprises a microcontroller, an input device, a communication module, a D/A converter, an electrothermal actuator and an A/D converter, wherein the input device, the communication module, the D/A converter and the A/D converter are connected with the microcontroller, the D/A converter is connected with the electrothermal actuator, the electrothermal actuator is connected with a heating element of the transmission line for the combination of gas chromatograph and mass spectrometer as claimed in claim 1, and the A/D converter is connected with a temperature sensor of the transmission line for the combination of gas chromatograph and mass spectrometer.
8. The apparatus of claim 7, wherein: the electrothermal actuator comprises an inverter and a solid-state relay, the microcontroller is connected with the inverter through the D/A converter, the inverter is connected with the solid-state relay, and the solid-state relay is connected with the heating element;
the display and the alarm device are connected with the microcontroller.
9. The utility model provides a gas chromatograph and mass spectrograph allies oneself with uses accuse temperature transmission line which characterized in that: the combined transmission line for gas chromatograph and mass spectrometer according to any one of claims 1 to 6, and the combined device for gas chromatograph and mass spectrometer according to any one of claims 7 to 8.
10. The method of claim 9, comprising the steps of:
calculating the temperature difference between the set transmission line temperature and the acquired current transmission line temperature;
calculating a duty ratio according to the calculated temperature difference;
controlling the heating rate of the heating element according to the calculated duty ratio, and controlling the heating element to heat at a first heating rate when the acquired current temperature of the transmission line is lower than a temperature threshold value; when the acquired current temperature of the transmission line is not lower than the temperature threshold, controlling the heating element to heat at a second heating rate; wherein the first heating rate is greater than the second heating rate.
CN202210900178.6A 2022-07-28 2022-07-28 Transmission line and device for combined use of gas chromatograph and mass spectrometer, temperature control transmission line and method Pending CN115308324A (en)

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Citations (9)

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