CN217655064U

CN217655064U - Thermal cracking chromatographic detector

Info

Publication number: CN217655064U
Application number: CN202221249587.6U
Authority: CN
Inventors: 刘钟
Original assignee: Beijing Jsdy Analytical Instruments R & D Center
Current assignee: Beijing Jsdy Analytical Instruments R & D Center
Priority date: 2022-05-23
Filing date: 2022-05-23
Publication date: 2022-10-25
Anticipated expiration: 2032-05-23

Abstract

The utility model relates to a thermal cracking chromatogram detector, it includes: vertical direction is equipped with the baffle in the device shell, and the top surface is equipped with sampling device, the baffle with be provided with the instrument board in the device shell one side inner wall formative space, sampling device includes: the thermal cracker is communicated with the sample injector, the sample injector is communicated with the chromatographic column, a back-blowing outlet is arranged on the thermal cracker, a load valve plate is arranged on a partition plate, a carrier gas inlet is arranged on a shell of the device and is connected with a pressure stabilizing valve I, an outlet of the pressure stabilizing valve I is connected with a pressure gauge I, the pressure stabilizing valve I is divided into two gas path outlets after passing through a three-way valve, the two gas path outlets are respectively communicated with a gas pipe I and a gas pipe II, the gas pipe I is connected with a switch valve I and is communicated with the thermal cracker to form a gas path structure, the gas pipe II is connected with the switch valve II and is communicated with the sample injector to form the gas path structure, and the gas paths of the thermal cracker and the chromatographic detection are shared, so that the whole pipeline is reasonably planned and designed in a box body, the size of the device is reduced, and the experimental space is saved.

Description

Thermal cracking chromatographic detector

The technical field is as follows:

the utility model relates to a chromatogram detector, especially a thermal cracking chromatogram detector.

Background

The pyrolysis gas chromatography is a common chromatography detection method and has a wide application field, but because the thermal cracking instrument and the gas chromatograph belong to different equipment, the gas path is long and complex in the mutual connection between the two equipment, and a large amount of redundancy exists in the pipeline volume, so that the dead volume and the failure rate are increased invisibly.

For example, the name "a portable thermal cracking gas chromatograph", publication number: in view of the disclosure in the technical scheme of CN209784285U, the novel technical scheme is used to specifically solve the problems of on-site acquisition, detection and data collection, and specifically uses a thermal cracking gas chromatograph including: a portable gas chromatograph, a thermal cracking instrument and a sample inlet converter; the thermal cracking instrument is connected with the portable gas chromatograph through the sample inlet converter. However, the method still cannot be used for separating a chromatograph and a thermal cracking instrument into two instruments.

Also named as 'a special gas chromatograph for rapidly determining the material of the plastic food bag', the publication number is: the technical scheme of CN202814936U discloses that it uses a novel technical scheme to rapidly and conveniently measure the material type of plastic food bags, and uses a gas chromatograph, which includes a mainframe case, a networked electronic control system with a built-in chromatographic workstation, an internal flow-dividing capillary chromatographic column sample injector, a corresponding gas circuit control system, a flame ionization detector, a capillary chromatographic column, and a tube furnace cracker, whose output component is connected with the internal flow-dividing capillary chromatographic column sample injector. However, the present invention cannot solve the problem of integration of a thermal cracker and a chromatograph, and the present invention is particularly proposed in view of this.

SUMMERY OF THE UTILITY MODEL

In order to solve the technical problem, the utility model discloses a thermal cracking chromatography detector, it includes: the device comprises a device shell, wherein a partition board is arranged in the device shell in the vertical direction, a sample feeding device is arranged on the top surface of the device shell, and an instrument board is arranged in a space formed by the partition board and the inner wall of one side of the device shell;

the sampling device comprises: the thermal cracker is communicated with the sample injector, and the sample injector is communicated with the chromatographic column to form a gas passage structure;

the thermal cracker is provided with a back-blowing outlet, and forms a gas passage structure with the external atmosphere through a gas pipe III, and the gas pipe III is connected with a switch valve III; a pressure stabilizing valve I and a pressure gauge I are arranged on the instrument board;

the partition plate is provided with a load valve plate, the load valve plate protrudes out of the partition plate through a support nail, a space is reserved between the load valve plate and the partition plate, and the load valve plate is provided with a switch valve I, a switch valve II and a switch valve III;

the device comprises a shell, a pressure stabilizing valve I, a pressure stabilizing valve II, a gas pipe I, a switch valve I, a thermal cracker and a gas injector, wherein a carrier gas inlet is formed in the shell of the device and connected with the pressure stabilizing valve I, one outlet of the pressure stabilizing valve I is connected with the pressure gauge I, the other outlet of the pressure stabilizing valve I is connected with the three-way valve and is divided into two gas path outlets after passing through the three-way valve, the two gas path outlets are respectively communicated with the gas pipe I and the gas pipe II, the gas pipe I is connected with the switch valve I and is communicated with the thermal cracker to form a gas passage structure, and the gas pipe II is connected with the switch valve II and is communicated with the injector to form a gas passage structure.

Specifically, the thermal cracker includes the sampling pipe, and the heating member cover is established on the sampling pipe, sampling pipe one end is connected with a kind sealing joint, and forms gas tightness gas passage through a kind sealing joint and trachea I, the injector is including annotating the appearance pipe, annotating the sealed intercommunication of the one end of appearance pipe and the other end of sampling pipe, make advance a kind sealing joint, sampling pipe and annotate appearance pipe three and form the route structure, annotate the appearance pipe other end and communicate with the chromatographic column as annotating a kind export.

Specifically, the switch valve I, the switch valve II and the switch valve III are mechanical switch valves;

specifically, the joints of the air pipes I, II and III and the switch valve are hoses.

Specifically, the air pipe I is communicated with the thermal cracker, the air pipe II is communicated with the injector, and the joint of the air pipe I and the injector is a hard pipe.

Specifically, the top surface of the device shell is also provided with a detector, and the detector is connected with an outlet of the chromatographic column.

Specifically, a gas inlet I and a gas inlet II are arranged on the device shell; the instrument panel is further provided with a pressure stabilizing valve II, a pressure stabilizing valve III, a pressure gauge II and a pressure gauge III, the pressure stabilizing valve II is connected with the air inlet I, the outlet of the pressure stabilizing valve II is respectively connected with the pressure gauge II and the detector, the pressure stabilizing valve III is connected with the air inlet II, and the outlet of the pressure stabilizing valve III is respectively connected with the pressure gauge III and the detector.

Specifically, the thermal cracking chromatographic detector further comprises a tail blowing needle valve arranged on the instrument panel, one end of the tail blowing needle valve is connected with a connecting channel between the carrier gas inlet and the pressure stabilizing valve I, and the other end of the tail blowing needle valve is connected with the tail end of the chromatographic column and arranged on the connecting channel between the chromatographic column and the detector.

Specifically, the thermal cracking chromatographic detector further comprises a flow divider valve arranged on the instrument panel and connected with the sample injector to form a structure communicated with the external atmosphere through a pipeline.

Advantageous effects

The utility model provides a thermal cracking chromatograph, its advantage effect has:

1. the gas circuit sharing of thermal cracking and chromatogram detection plans and designs holistic pipeline in the box is reasonable, has reduced the volume of equipment, has saved the experimental space.

2. The sampling device shortens the sampling distance, improves the efficiency of thermal cracking, reduces the dead volume in the sampling device and improves the detection accuracy.

Drawings

FIG. 1 is a schematic structural diagram of a thermal cracking chromatography detector according to the present invention;

FIG. 2 is a schematic structural diagram of a thermal cracking chromatography detector according to the present invention;

fig. 3 is a schematic view of the sample feeding device of the present invention.

Legend: 1. a device housing; 11. a carrier gas inlet; 12. a gas inlet I; 13. a gas inlet II; 2. a sample introduction device; 21. a thermal cracker; 211. a sampling tube; 212. a heating body; 213. a sample introduction sealing joint; 22. a sample injector; 221. injecting a sample tube; 3. a partition plate; 31. a valve-carrying plate; 311. a support pin; 4 an instrument panel; 41A, a pressure maintaining valve I;41B and a pressure stabilizing valve II;41C, a pressure maintaining valve III;42A and a pressure gauge I;42B, a pressure gauge II;42C, a pressure gauge III;43A, a switch valve I;43B switching valve II;43C, a switch valve III;44A, trachea I;44B, a trachea II;44C, trachea III; 45. a tail blow needle valve; 46. a flow divider valve; 5, a chromatographic column; 6. a detector.

Detailed Description

The present invention is further illustrated by the following examples, but is not limited to the contents of the specification.

A thermal cracking chromatography detector as shown in fig. 1 and 2, comprising: device shell 1, vertical direction is equipped with baffle 3 in the device shell 1, and the top surface is equipped with sampling device 2, is provided with instrument board 4 in baffle 3 and the 1 one side inner wall formation space of device shell, forms a space in device shell 1, concentrates the gas circuit to set up in this space, reduces the whole pipeline of gas circuit, saves tubular product, and sampling device 2 includes: the thermal cracker 21 is communicated with the injector 22, and the injector 22 is communicated with the chromatographic column 5 to form a gas passage structure; a blowback outlet is arranged on the thermal cracker 21, a gas passage structure is formed with the external atmosphere through a gas pipe III44C, and the gas pipe III44C is connected with a switch valve III43C; be equipped with surge damping valve I41A on the instrument board 4, manometer I42A, sampling device 2 and chromatographic column 5 direct intercommunication, the sampling distance between sampling device 2 and the chromatographic column 5 has been shortened, when the chromatogram is examined, the dead volume in the pipeline has been reduced, can effectually wait to detect gas and blow into chromatographic column 5, improve the accuracy of testing result, in the chromatogram experiment, need wash the pipeline after detecting the completion, can discharge unnecessary liquid solvent when detecting liquid solvent, solvent peak is too big when avoiding detecting, influence the testing result, through setting up the blowback export, can wash the pipeline, discharge solvent liquid, can also play the guard action to the pipeline.

The partition plate 3 is provided with a load valve plate 31, the load valve plate 31 protrudes out of the partition plate 3 through a support nail 311, a distance is reserved between the load valve plate and the partition plate 3, and the load valve plate is provided with a switch valve I43A, a switch valve II43B and a switch valve III43C; in the chromatogram detection experiment, the condition that the pipeline needs to be replaced and the equipment needs to be overhauled can appear, and the valve plate 31 is arranged by protruding the partition plate 3, so that the replacement and the inspection of the switch valve and the pipeline can be carried out through the distance between the switch valve and the pipeline when the equipment is overhauled.

The device comprises a device shell 1, a carrier gas inlet 11 is arranged on the device shell 1 and connected with a pressure stabilizing valve I41A, one outlet of the pressure stabilizing valve I41A is connected with a pressure gauge I42A, the other outlet of the pressure stabilizing valve I41A is connected with a three-way valve and is divided into two gas path outlets after passing through the three-way valve, a gas pipe I44A and a gas pipe II44B are respectively communicated, the gas pipe I44A and a switch valve I43A are connected and communicated with a thermal cracker 21 to form a gas path structure, the gas pipe II44B is connected with a switch valve II43B and communicated with a sample injector 22 to form a gas path structure, the thermal cracking and chromatographic detection are integrated by the design, the gas paths of a thermal cracking and chromatographic detection system are shared, the whole pipeline is reasonably planned and designed in a box body, the size of equipment is reduced, and the experimental space is saved.

In order to further shorten the gas path of the thermal cracking chromatographic detector, as shown in fig. 3, the sample injection device 2 includes a thermal cracking device 21 including a sampling tube 211, a heating body 212 is sleeved on the sampling tube 211, one end of the sampling tube 211 is connected with a sample injection sealing joint 213, and an airtight gas passage is formed with a gas pipe I44A through the sample injection sealing joint 213, the sample injector 22 includes a sample injection tube 221, one end of the sample injection tube 221 is in sealing communication with the other end of the sampling tube 211, so that the sample injection sealing joint 213, the sampling tube 211 and the sample injection tube 221 form a passage structure, the other end of the sample injection tube 221 is used as a sample injection outlet to be communicated with the chromatographic column 5, the sample injection tube 221 is communicated with the sample injection tube 221 to form an airtight gas passage, when the sample injection sealing joint 213 is opened, a solid or liquid or gas sample is directly injected, the sample can be rapidly dropped to the bottom of the sample injection tube 211, the sample injection distance is shortened, the efficiency of the sample injection tube is improved, the sample is instantaneously cracked at a constant thermal cracking temperature after reaching the thermal cracking tube 21, thereby ensuring that the sample remains a stable state after the sample is cracked, when the sealing communication is detected, the sample injection tube 221 can be fully carried, and the secondary cracking reaction in the sample injection tube is greatly reduced.

Carry ooff valve I43A on the valve plate 31, ooff valve II43B, ooff valve III43C is mechanical ooff valve, mechanical valve sets up towards 1 curb plate direction of device shell, mechanical valve's simple structure, long service life, mechanical valve separates mutually with baffle 3 through carrying valve plate 31, be convenient for install and overhaul, to changing in equipment and the maintenance equipment can quick replacement, and can cooperate opening and closing of better realization gas circuit with the trachea.

Trachea I44A, trachea II44B, trachea III44C are the hose with the ooff valve junction, carry and are equipped with the through-hole on the valve plate 31, and the trachea is worn out through the through-hole and is carried the valve plate in through carrying the interval between valve plate 31 and the baffle 3 to fixed with the mechanical valve, the trachea for the hose can be better cooperate with the mechanical valve, reach opening and closing of control gas circuit.

The air pipe I44A is communicated with the thermal cracker 21, the air pipe II44B is communicated with the injector 22, the joint is a hard pipe, the thermal cracker 21 and the injector 22 need to be heated during chromatographic detection, the air pipe at the joint is a hard pipe, impurities are prevented from being generated during heating, and the detection result is prevented from being influenced, and the air pipe I44A and the air pipe II44B are provided with conversion valves, so that the air pipe passing through the mechanical valve is converted into the hard pipe.

The top surface of the device shell 1 is also provided with a detector 6, the detector 6 is connected with the outlet of the chromatographic column 5, the detector 6 can be a hydrogen flame ion detector, and the detector 6 can detect the gas separated by the chromatographic column 5 to complete the chromatographic detection step.

The device shell 1 is provided with a gas inlet I12 and a gas inlet II13; the instrument panel is also provided with a pressure stabilizing valve II41B, a pressure stabilizing valve III41C, a pressure gauge II42B and a pressure gauge III42C, the pressure stabilizing valve II41B is connected with a gas inlet I12, an outlet is respectively connected with the pressure gauge II42B and the detector 6, the pressure stabilizing valve III41C is connected with a gas inlet II13, an outlet is respectively connected with the pressure gauge III42C and the detector 6, the gas inlet I12 and the gas inlet II13 provide combustion-supporting gas for the detector 6, the gas inlet is connected with the pressure stabilizing valve and the pressure gauge, the pressure value of gas during detection can be clearly displayed, effective data is provided for detection, the pressure stabilizing valve II41B and the pressure stabilizing valve III41C provide stable pressure for the subsequent detection process of the gas, the stability of the total flow of a sample inlet is ensured, and then the stable detection pressure is ensured.

The thermal cracking chromatographic detector also comprises a tail blowing needle valve 45 which is arranged on the instrument board 4, one end of the tail blowing needle valve is connected with a connecting channel of the carrier gas inlet 11 and the pressure stabilizing valve I41A, the other end of the tail blowing needle valve is connected with the tail end of the chromatographic column and is arranged on the connecting channel of the chromatographic column 5 and the detector 6, when the chromatographic detector detects the chromatogram, the post dead volume is arranged at the connecting part between the chromatographic column 5 and the detector 6, the peak shape display of a detection result can be influenced, the tail blowing needle valve can enable gas to be detected to quickly reach the detector, the post dead volume is eliminated, the high-sensitivity work of the detector is ensured, and the detection result is more accurate.

The thermal cracking chromatographic detector also comprises a shunt valve 46 which is arranged on the instrument panel 4 and connected with the sample injector 22 to form a structure communicated with the outside atmosphere through a pipeline, the shunt valve can place overload of a sample, when a sample solvent is injected, solvent liquid and a solute to be detected are introduced into the thermal cracking device 21 for cracking desorption, in the process, the sample gas to be detected can be filled in the sample injector 2, the column capacity of the chromatographic column 5 is not enough to support all the gas to be detected to enter the chromatographic column, the shunt valve can relieve the detection pressure of the chromatographic column 5, and adverse effects such as widening of the peak shape of the detection result of the chromatographic column are avoided.

It is to be understood that the above-described embodiments of the present invention are merely examples provided for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. Not all embodiments are exhaustive. All obvious changes or variations led out by the technical scheme of the utility model are still in the protection scope of the utility model.

Claims

1. A thermal cracking chromatography detector, comprising: the device comprises a device shell (1), wherein a partition plate (3) is arranged in the device shell (1) in the vertical direction, a sample feeding device (2) is arranged on the top surface of the device shell, and an instrument panel (4) is arranged in a space formed by the partition plate (3) and the inner wall of one side of the device shell (1);

the sample introduction device (2) comprises: the thermal cracker (21) is communicated with the injector (22), and the injector (22) is communicated with the chromatographic column (5) to form a gas passage structure;

a back flushing outlet is arranged on the thermal cracker (21), a gas passage structure is formed with the external atmosphere through a gas pipe III (44C), and the gas pipe III (44C) is connected with a switch valve III (43C);

a pressure stabilizing valve I (41A) and a pressure gauge I (42A) are arranged on the instrument panel (4);

the partition plate (3) is provided with a load valve plate (31), the load valve plate (31) protrudes out of the partition plate (3) through a support nail (311) and is arranged at a distance, and the load valve plate is provided with a switch valve I (43A), a switch valve II (43B) and a switch valve III (43C);

be equipped with carrier gas entry (11) on device shell (1), the carrier gas entry is connected with pressure-stabilizing valve I (41A), and pressure-stabilizing valve I (41A) exit linkage manometer I (42A), another exit linkage three way valve door divide into two gas circuit exports behind the three way valve door, communicate trachea I (44A) and trachea II (44B) respectively, trachea I (44A) is connected with ooff valve I (43A), and communicates with thermal cracker (21) and form the gas path structure, trachea II (44B) are connected with ooff valve II (43B), and communicate with injector (22) and form the gas path structure.

2. A thermal cracking chromatography detector according to claim 1, wherein: thermal cracker (21) are established on sampling tube (211) including sampling tube (211), heating body (212) cover, sampling tube (211) one end is connected with into appearance sealing joint (213), and forms gas tightness gas passage through into appearance sealing joint (213) and trachea I (44A), annotate appearance ware (22) including annotating appearance pipe (221), the one end of annotating appearance pipe (221) and the other end of sampling tube (211) seal the intercommunication, make and advance appearance sealing joint (213), sampling tube (211) and annotate appearance pipe (221) three and form the access structure, annotate appearance pipe (221) other end and communicate with chromatographic column (5) as annotating the appearance export.

3. A thermal cracking chromatography detector according to claim 1, wherein: and the switch valve I (43A), the switch valve II (43B) and the switch valve III (43C) are mechanical switch valves.

4. A thermal cracking chromatography detector according to claim 1, wherein: the joints of the air pipe I (44A), the air pipe II (44B), the air pipe III (44C) and the switch valve are hoses.

5. A thermal cracking chromatography detector according to claim 4, wherein: the air pipe I (44A) is communicated with the thermal cracker (21), the air pipe II (44B) is communicated with the injector (22), and the joint of the air pipe I and the air pipe II is a hard pipe.

6. A thermal cracking chromatography detector according to claim 1, wherein: the top surface of the device shell (1) is also provided with a detector (6), and the detector (6) is connected with the outlet of the chromatographic column (5).

7. A thermal cracking chromatography detector according to claim 1, wherein: the device shell (1) is provided with an air inlet I (12) and an air inlet II (13);

a pressure stabilizing valve II (41B), a pressure stabilizing valve III (41C), a pressure gauge II (42B) and a pressure gauge III (42C) are also arranged on the instrument panel,

the pressure stabilizing valve II (41B) is connected with the gas inlet I (12), the outlet is respectively connected with the pressure gauge II (42B) and the detector (6),

and the pressure stabilizing valve III (41C) is connected with the gas inlet II (13), and the outlet is respectively connected with the pressure gauge III (42C) and the detector (6).

8. A thermal cracking chromatograph according to claim 1, wherein: the device also comprises a tail-blowing needle valve (45) which is arranged on the instrument panel (4), one end of the tail-blowing needle valve is connected with a connecting channel of the carrier gas inlet (11) and the pressure stabilizing valve I (41A), and the other end of the tail-blowing needle valve is connected with the tail end of the chromatographic column and is arranged on a connecting channel of the chromatographic column (5) and the detector (6).

9. A thermal cracking chromatography detector according to claim 1, wherein: the instrument panel is characterized by further comprising a diverter valve (46) which is arranged on the instrument panel (4) and connected with the sample injector (22) to form a structure communicated with the outside atmosphere through a pipeline.