CN112666296A - Dual-channel thermal desorption sampling system and method for chromatograph detection - Google Patents
Dual-channel thermal desorption sampling system and method for chromatograph detection Download PDFInfo
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- CN112666296A CN112666296A CN202110279355.9A CN202110279355A CN112666296A CN 112666296 A CN112666296 A CN 112666296A CN 202110279355 A CN202110279355 A CN 202110279355A CN 112666296 A CN112666296 A CN 112666296A
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Abstract
The invention discloses a dual-channel thermal desorption sample injection system and a method for chromatograph detection, wherein the dual-channel thermal desorption sample injection system for chromatograph detection comprises a primary desorption device, a secondary cold trap device A and a secondary cold trap device B, wherein the output end of the primary desorption device is provided with a gas path which is divided into a branch gas path A and a branch gas path B … …; a method of a dual-channel thermal desorption sampling system for chromatograph detection comprises the following steps: s1 dry blowing the primary desorption device, S2 releasing the target compound in the primary desorption device, S3 carrier gas carrying the target compound and introduced into the secondary cold trap device A through the branch gas path A to adsorb the target compound, and S2 operation releases the target compound … … in the primary desorption device.
Description
Technical Field
The invention relates to the technical field of sample detection and analysis, in particular to a dual-channel thermal desorption sampling system and a dual-channel thermal desorption sampling method for chromatograph detection.
Background
The thermal desorption sample injection technology is a sample injection technology which is widely applied at present. The thermal desorption sample introduction technology is widely applied to the fields of life science, industry, agriculture, environmental protection, pharmacy, tobacco, education, petrifaction, toxicology, food, electronics and the like. The main equipment of the thermal desorption sampling technology is a thermal desorption instrument. The thermal desorption sampling technology is that the solid sample or the adsorption tube with the substance to be detected is placed in a thermal desorption device, the device is directly connected with a chromatograph, and carrier gas enters a sample inlet of the chromatograph through the thermal desorption device. When the temperature of the thermal desorption device is increased, the volatile components are released from the solid sample or the adsorbent and enter a gas chromatographic system along with the carrier gas for analysis and determination.
The second-stage thermal desorption technology is that the target compound desorbed from the first-stage desorption tube is re-adsorbed in a subsequent gas path by a small amount of adsorbent and an electronic refrigeration technology (second-stage cold trap), the cold trap is focused, and the target component is desorbed again in a mode of instantly heating and purging the second-stage cold trap and is introduced into the gas chromatography. At the moment, the peak shape of the chromatogram is obviously narrowed, the separation degree is better, and the peak appearance performance is more excellent.
In the current technical environment, the development demand of the environmental VOC detection field is increased suddenly, and the analysis time of most of the detection methods of environmental VOC and TVOC reaches 1 hour, so that the working efficiency of the detection mechanism is greatly restricted. At present, the gas chromatograph can be configured with double injection ports and double detectors, and the traditional thermal desorption instrument only has one channel and can only enter one of the injection ports. Therefore, in order to improve the analysis efficiency of a user and reduce the purchase cost of the user, the invention provides a dual-channel thermal desorption sampling system and method for chromatograph detection.
Disclosure of Invention
The invention aims to provide a dual-channel thermal desorption sampling system and a dual-channel thermal desorption sampling method for chromatograph detection, so as to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme: the utility model provides a binary channels thermal desorption sampling system for chromatograph detects, includes one-level desorption device, second grade cold trap device A, second grade cold trap device B, one-level desorption device output is provided with the gas circuit, the gas circuit reposition of redundant personnel is branch gas circuit A and branch gas circuit B, branch gas circuit A connects second grade cold trap device A's input, branch gas circuit B connects second grade cold trap device B's input, chromatograph is all connected to second grade cold trap device A and second grade cold trap device B's output. The first-stage desorption device, the second-stage cold trap device A and the second-stage cold trap device B are all devices in the thermal desorption instrument, namely, a double-channel cold trap is arranged in the thermal desorption instrument, so that the thermal desorption instrument can be connected with two sample inlets of the same chromatograph or two different chromatographs; when the double-channel cold trap is connected with two sample inlets of the same chromatograph, the device can firstly use a first-stage desorption device to release a target compound, then use a second-stage cold trap device A to adsorb the target compound, then use the desorption device to release the target compound and the time difference of the cold trap device to adsorb the target compound, then use the first-stage desorption device to release the target compound, then use a second-stage cold trap device B to adsorb the target compound, finally desorb the target compound in the second-stage cold trap device A and the second-stage cold trap device B, and introduce the target compound into two sample inlets of the same chromatograph to carry out simultaneous analysis, so that one thermal desorption instrument and one chromatograph can be used for analyzing the target compound with the analysis amount twice that of the traditional thermal desorption system, and on the premise of greatly reducing the analysis time, the purchase cost of the equipment can; when the double-channel cold trap is connected with two different chromatographs, the device can firstly use the first-stage desorption device to release a target compound, then the released target compound is shunted into the second-stage cold trap device A and the second-stage cold trap device B to be adsorbed, then the target compound in the second-stage cold trap device A and the second-stage cold trap device B is desorbed, and the target compound is led into the two different chromatographs to be analyzed by two different methods of the same sample, and the advantages of reduced analysis time and reduced analysis cost can be achieved.
Preferably, the first-stage desorption device comprises a first-stage desorption transfer membrane valve, a carrier gas switch valve A, a carrier gas pressure detector, a precise pressure regulating valve and a first-stage desorption tube, the fourth end of the first-stage desorption transfer membrane valve is connected with the carrier gas switch valve A through a pipeline, the carrier gas switch valve A is used for controlling the switching of a carrier gas channel, one end, away from the first-stage desorption transfer membrane valve, of the carrier gas switch valve A is connected with the carrier gas pressure detector through a pipeline, the carrier gas pressure detector is used for detecting the pressure of carrier gas in the channel, one end, away from the carrier gas switch valve A, of the carrier gas pressure detector is connected with the precise pressure regulating valve through a pipeline, the precise pressure regulating valve is used for regulating the pressure of the carrier gas in the channel, the first-stage desorption tube is connected between the third end and the sixth end of the first-, and the fifth end of the first-stage desorption transfer membrane valve is connected with the gas circuit.
Preferably, the carrier gas pressure detector is further connected with a carrier gas switch valve B through a pipeline, the carrier gas switch valve B is used for controlling the opening and closing of a first-level dry blowing passage, the carrier gas switch valve B is connected with the first end of the first-level desorption transfer membrane valve through a pipeline, the second end of the first-level desorption transfer membrane valve is connected with a leakage detection pressure detector through a pipeline, the leakage detection pressure detector is used for detecting whether carrier gas leaks from the first-level dry blowing passage or not, the carrier gas is used for ensuring that the inside of the first-level desorption pipe is completely dried, one end, far away from the first-level desorption transfer membrane valve, of the leakage detection pressure detector is connected with a flow path selection switch valve A through a pipeline, one end, far away from the leakage detection pressure detector, of the flow path selection switch valve A is connected with a flow controller.
Preferably, the secondary cold trap device a comprises a six-way membrane valve a, a secondary cold trap a, a flow path selection switch valve B and a flow controller B, the first end of the six-way membrane valve a is connected with the branch gas path a, the second end of the six-way membrane valve a is connected with the secondary cold trap a through a pipeline between the third end and the sixth end, the secondary cold trap a is used for re-adsorbing a target compound carried by the carrier gas, the second end of the six-way membrane valve a is connected with the flow path selection switch valve B through a pipeline, the flow path selection switch valve B is used for controlling the opening and closing of the branch gas path a, one end of the flow path selection switch valve B, which is far away from the six-way membrane valve a, is connected with the flow controller B through a pipeline, and the flow controller B is used for controlling the flow of the.
Preferably, the fourth end of the six-way membrane valve a is connected with a carrier gas inlet passage a, and the fifth end of the six-way membrane valve a is connected with a chromatograph.
Preferably, the secondary cold trap device B comprises a six-way membrane valve B, a secondary cold trap B, a flow path selection switch valve C and a flow controller C, the first end of the six-way membrane valve B is connected with the branch gas path B, the second end of the six-way membrane valve B is connected with the secondary cold trap B through a pipeline between the third end and the sixth end, the secondary cold trap B is used for re-adsorbing a target compound carried by carrier gas, the second end of the six-way membrane valve B is connected with the flow path selection switch valve C through a pipeline, the flow path selection switch valve C is used for controlling the opening and closing of the branch gas path B, one end of the flow path selection switch valve C, which is far away from the six-way membrane valve B, is connected with the flow controller C through a pipeline, and the flow controller C is used for controlling the flow of.
Preferably, the fourth end of the six-way membrane valve B is connected to the carrier gas inlet passage B, and the fifth end of the six-way membrane valve B is connected to the chromatograph.
Preferably, the air path, the branch air path a and the branch air path B are integrally formed. The gas path divides the carrier gas to enter the branch gas path A and the branch gas path B, and the branch gas path A and the branch gas path B are controlled by the flow path selection switch valve B and the flow path selection switch valve C, but not by arranging a valve at the division position, so that the gas path, the branch gas path A and the branch gas path B are integrally formed, the object to be detected can be kept from being polluted by the valve, and the detection precision is ensured.
Preferably, the method for the dual-channel thermal desorption sampling system for chromatograph detection comprises the following steps:
s1, carrying out dry blowing on a primary desorption device;
s2, releasing the target compound in the primary desorption device;
s3, introducing the carrier gas carrying the target compound into the secondary cold trap device A through the branch gas circuit A to adsorb the target compound, and simultaneously operating the step S2 to release the target compound in the primary desorption device;
s4, introducing the carrier gas carrying the target compound into the secondary cold trap device B through the branch gas circuit B to adsorb the target compound, and simultaneously operating the step S2 to release the target compound in the primary desorption device again;
s5, dry blowing is carried out on the secondary cold trap device A and the secondary cold trap device B;
and S6, desorbing the target compounds in the secondary cold trap device A and the secondary cold trap device B, and simultaneously introducing the target compounds into two analysis pipelines of a chromatograph for analysis and determination.
According to the method, the time difference between the target compound released by the desorption device and the target compound adsorbed by the cold trap device is utilized, the target compounds in the secondary cold trap device A and the secondary cold trap device B are desorbed and are introduced into two sample inlets of the same chromatograph for simultaneous analysis, the target compounds with the analysis amount twice that of the traditional thermal desorption system can be analyzed by using one thermal desorption instrument and one chromatograph, and the purchase cost of equipment can be reduced on the premise of greatly reducing the analysis time.
Preferably, the method for the dual-channel thermal desorption sampling system for chromatograph detection comprises the following steps:
s1, carrying out dry blowing on a primary desorption device;
s2, releasing the target compound in the primary desorption device;
s3, introducing the carrier gas carrying the target compound into a secondary cold trap device A and a secondary cold trap device B through a branch gas circuit A and a branch gas circuit B respectively, and adsorbing the target compound by the secondary cold trap device A and the secondary cold trap device B;
s4, dry blowing is carried out on the secondary cold trap device A and the secondary cold trap device B;
and S5, desorbing the target compounds in the secondary cold trap device A and the secondary cold trap device B, and simultaneously introducing the target compounds into two analysis pipelines of a chromatograph for analysis and determination.
According to the method, after the target compounds in the secondary cold trap device A and the secondary cold trap device B are desorbed, the target compounds are simultaneously introduced into the two analysis pipelines of the chromatograph for analysis and determination, the purchase cost of equipment can be reduced on the premise of reducing the analysis time, the target compounds can also be introduced into two different chromatographs for analysis of the same sample by two different methods, and the advantages of reducing the analysis time and the analysis cost can also be achieved.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention discloses a dual-channel thermal desorption sample injection system and a method for chromatograph detection, wherein a dual-channel cold trap is arranged in a thermal desorption instrument, so that the thermal desorption instrument can be connected with two sample injection ports of the same chromatograph, when thermal desorption analysis is carried out, the device can firstly use a first-stage desorption device to release a target compound, then use a second-stage cold trap device A to adsorb the target compound, then use the desorption device to release the time difference between the target compound and the cold trap device to adsorb the target compound, then use the first-stage desorption device to release the target compound, then use a second-stage cold trap device B to adsorb the target compound, finally desorb the target compound in the second-stage cold trap device A and the second-stage cold trap device B, introduce the target compound into the two sample injection ports of the same chromatograph to carry out simultaneous analysis, thus use one thermal desorption instrument and one chromatograph to analyze the target compound with the analysis amount twice as that of, on the premise of greatly reducing the analysis time, the purchase cost of equipment can be reduced;
2. the invention discloses a dual-channel thermal desorption sample introduction system and a method for chromatograph detection.A dual-channel cold trap is arranged in a thermal desorption instrument, so that the thermal desorption instrument can be connected with two sample inlets of the same chromatograph, when thermal desorption analysis is carried out, the device can firstly use a first-stage desorption device to release a target compound, then the released target compound is shunted into a second-stage cold trap device A and a second-stage cold trap device B to be adsorbed, then the target compound in the second-stage cold trap device A and the second-stage cold trap device B is desorbed, and the target compound is introduced into two different chromatographs to be analyzed by two different methods of the same sample, and the advantages of reduced analysis time and analysis cost can also be achieved;
3. the invention discloses a dual-channel thermal desorption sampling system for chromatograph detection, which is characterized in that after carrier gas carries a target compound released by a primary desorption device, the carrier gas is divided into a branch gas circuit A and a branch gas circuit B in a gas circuit and is controlled by a flow path selection switch valve B and a flow path selection switch valve C instead of a valve at the division position, so that the gas circuit, the branch gas circuit A and the branch gas circuit B are integrally formed, an object to be detected can be kept from being polluted by the valve, and the detection precision is ensured.
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 specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic diagram of a dual-channel thermal desorption sampling system for chromatograph detection according to the present invention;
FIG. 2 is a schematic view of step S1 in example 1 of the present invention;
FIG. 3 is a schematic view of step S2 in example 1 of the present invention;
FIG. 4 is a schematic view of step S3 in embodiment 1 of the present invention;
FIG. 5 is a schematic view of step S4 in example 1 of the present invention;
FIG. 6 is a schematic view of step S5 in embodiment 1 of the present invention;
FIG. 7 is a schematic view of step S6 in embodiment 1 of the present invention;
fig. 8 is a schematic view of step S1 in embodiment 2 of the present invention;
fig. 9 is a schematic view of step S2 in embodiment 2 of the present invention;
fig. 10 is a schematic view of step S3 in embodiment 2 of the present invention;
fig. 11 is a schematic view of step S4 in embodiment 2 of the present invention;
fig. 12 is a schematic view of step S5 in embodiment 2 of the present invention;
in the figure: a first-order desorption device-1; a secondary cold trap device A-2; a secondary cold trap device B-3; a gas circuit-4; a branch gas circuit A-5; a branch gas circuit B-6; a first-order desorption transfer membrane valve-7; a carrier gas switch valve A-8; a carrier gas pressure detector-9; a precision pressure regulating valve-10; a first-stage desorption pipe-11; a carrier gas switch valve B-12; a leak detection pressure detector-13; a flow path selection switch valve A-14; a flow controller A-15; a six-way membrane valve A-16; a secondary cold trap A-17; a carrier gas inlet A-18; a flow path selection switch valve B-19; a flow controller B-20; a six-way membrane valve B-21; a secondary cold trap B-22; a carrier gas inlet B-23; a flow path selection switch valve C-24; and a flow controller C-25.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides the technical scheme that: as fig. 1, a binary channels thermal desorption sampling system for chromatograph detects, including one-level desorption device 1, second grade cold trap device A2, second grade cold trap device B3, one-level desorption device 1 output is provided with gas circuit 4, gas circuit 4 reposition of redundant personnel is branch gas circuit A5 and branch gas circuit B6, branch gas circuit A5 connects second grade cold trap device A2's input, branch gas circuit B6 connects the input of second grade cold trap device B3, chromatograph is all connected to second grade cold trap device A2 and second grade cold trap device B3's output. The first-stage desorption device 1, the second-stage cold trap device A2 and the second-stage cold trap device B3 are all devices in the thermal desorption instrument, namely, a double-channel cold trap is arranged in the thermal desorption instrument, so that the thermal desorption instrument can be connected with two sample inlets of the same chromatograph and also can be connected with two different chromatographs; when the double-channel cold trap is connected with two sample inlets of the same chromatograph, the device can firstly use the first-stage desorption device 1 to release a target compound, then use the second-stage cold trap device A2 to adsorb the target compound, then use the desorption device to release the time difference between the target compound and the cold trap device to adsorb the target compound, then use the first-stage desorption device 1 to release the target compound again, then use the second-stage cold trap device B3 to adsorb the target compound, finally desorb the target compound in the second-stage cold trap device A2 and the second-stage cold trap device B3, introduce the target compound into two sample inlets of the same chromatograph to carry out simultaneous analysis, thus use one thermal desorption instrument and one chromatograph to analyze the target compound with the analysis amount twice that of the traditional thermal desorption system, and on the premise of greatly reducing the analysis time, also can reduce the purchase cost of the equipment; when the dual-channel cold trap is connected with two different chromatographs, the device can firstly use the first-stage desorption device 1 to release a target compound, then the released target compound is shunted into the second-stage cold trap device A2 and the second-stage cold trap device B3 to be adsorbed, then the target compound in the second-stage cold trap device A2 and the second-stage cold trap device B3 is desorbed, and the target compound is led into the two different chromatographs to be analyzed by two different methods of the same sample, and the advantages of reduced analysis time and reduced analysis cost can be achieved.
The primary desorption device 1 comprises a primary desorption transfer membrane valve 7, a carrier gas switch valve A8, a carrier gas pressure detector 9, a precise pressure regulating valve 10 and a primary desorption tube 11, wherein the fourth end of the primary desorption transfer membrane valve 7 is connected with the carrier gas switch valve A8 through a pipeline, the carrier gas switch valve A8 is used for controlling the switching of a carrier gas passage, one end, away from the primary desorption transfer membrane valve 7, of the carrier gas switch valve A8 is connected with the carrier gas pressure detector 9 through a pipeline, the carrier gas pressure detector 9 is used for detecting the pressure of carrier gas in the passage, one end, away from the carrier gas switch valve A8, of the carrier gas pressure detector 9 is connected with the precise pressure regulating valve 10 through a pipeline, the precise pressure regulating valve 10 is used for regulating the pressure of carrier gas in the passage, and the primary desorption tube 11 is connected between the third end and the sixth end of the primary desorption, the first-stage desorption pipe 11 is internally provided with a sample to be detected, and the fifth end of the first-stage desorption transfer membrane valve 7 is connected with the gas circuit 4.
The carrier gas pressure detector 9 is also connected with a carrier gas switch valve B12 through a pipeline, the carrier gas switch valve B12 is used for controlling the switch of a primary dry blowing passage, the carrier gas switch valve B12 is connected with the first end of the first-stage desorption transfer membrane valve 7 through a pipeline, the second end of the first-stage desorption transfer membrane valve 7 is connected with a leak detection pressure detector 13 through a pipeline, the leak detection pressure detector 13 is used for detecting whether carrier gas leaks in the primary dry blowing passage, for ensuring the complete drying of the inside of the primary desorption pipe 11, one end of the leak detection pressure detector 13 far away from the primary desorption transfer membrane valve 7 is connected with a flow path selection switch valve A14 through a pipeline, the flow path selection switch valve a14 is connected to a flow controller a15 through a pipe at the end remote from the leak detection pressure detector 13, and the flow controller a15 is used for controlling the pressure of the carrier gas in the primary dry blow passage.
The secondary cold trap device A2 comprises a six-way membrane valve A16, a secondary cold trap A17, a flow path selection switch valve B19 and a flow controller B20, wherein a first end of the six-way membrane valve A16 is connected with a branch gas path A5, a second cold trap A17 is connected between a third end and a sixth end of the six-way membrane valve A16 through a pipeline, the secondary cold trap A17 is used for re-adsorbing a target compound carried by carrier gas, a second end of the six-way membrane valve A16 is connected with a flow path selection switch valve B19 through a pipeline, the flow path selection switch valve B19 is used for controlling the opening and closing of the branch gas path A5, one end, far away from the six-way membrane valve A16, of the flow path selection switch valve B19 is connected with a flow controller B20 through a pipeline, and the flow controller B20 is used for controlling the flow size of the carrier gas in the.
The fourth end of the six-way membrane valve A16 is connected with a carrier gas inlet A18, and the fifth end of the six-way membrane valve A16 is connected with a chromatograph. The process of analyzing and measuring the target compound desorbed by the secondary cold trap device A2 comprises the following steps: and opening a six-way membrane valve A16, allowing the carrier gas to enter a secondary cold trap A17 through a carrier gas inlet A18, and allowing the carrier gas to carry the target compound in the secondary cold trap A17 into a chromatograph for analysis and determination.
The secondary cold trap device B3 comprises a six-way membrane valve B21, a secondary cold trap B22, a flow path selection switch valve C24 and a flow controller C25, wherein a first end of the six-way membrane valve B21 is connected with a branch gas path B6, a second cold trap B22 is connected between a third end and a sixth end of the six-way membrane valve B21 through a pipeline, the secondary cold trap B22 is used for re-adsorbing a target compound carried by carrier gas, a second end of the six-way membrane valve B21 is connected with a flow path selection switch valve C24 through a pipeline, the flow path selection switch valve C24 is used for controlling the opening and closing of the branch gas path B6, one end, far away from the six-way membrane valve B21, of the flow path selection switch valve C24 is connected with a flow controller C25 through a pipeline, and the flow controller C25 is used for controlling the flow size of the carrier gas in the.
The fourth end of the six-way membrane valve B21 is connected with a carrier gas inlet B23, and the fifth end of the six-way membrane valve B21 is connected with a chromatograph.
The air passage 4, the branch air passage A5 and the branch air passage B6 are integrally formed. The gas path 4 divides the carrier gas to enter the branch gas path A5 and the branch gas path B6 and controls the carrier gas through the flow path selection switch valve B19 and the flow path selection switch valve C24 instead of arranging a valve at the division position, so that the gas path 4, the branch gas path A5 and the branch gas path B6 are integrally formed, the object to be detected can be kept from being polluted by the valve, and the detection precision is ensured.
Example 1: a method for a dual-channel thermal desorption sampling system for chromatograph detection comprises the following steps:
s1, carrying out dry blowing on a primary desorption device 1, which comprises the following specific steps:
as shown in fig. 2, the carrier gas switch valve B12 and the flow path selection switch valve a14 are opened, the carrier gas is introduced into the primary desorption pipe 11 through the carrier gas switch valve B12, the dried carrier gas reversely purges the primary desorption pipe 11 to carry out moisture in the primary desorption pipe 11, and the flow controller a15 controls the flow rate of the primary dry blowing.
S2, releasing the target compound in the first-stage desorption device 1, which comprises the following specific steps:
as shown in fig. 3, the first-stage desorption/transfer membrane valve 7 and the carrier gas switch valve A8 are opened, the first-stage desorption/suction pipe 11 is heated to release the target compound adsorbed in the first-stage desorption/suction pipe 11, the carrier gas enters the first-stage desorption/suction pipe 11 through the precision pressure regulating valve 10, the carrier gas pressure detector 9 and the carrier gas switch valve A8, and the released target compound is carried into the gas path 4.
S3, introducing the target compound carried by the carrier gas into a secondary cold trap device A2 through a branch gas circuit A5 to adsorb the target compound, and simultaneously operating the step S2 to release the target compound in the primary desorption device 1, wherein the specific steps are as follows:
as shown in fig. 4, the six-way membrane valve a16 and the flow path selection switch valve B19 are opened, the carrier gas carrying the target compound in the gas path 4 enters the secondary cold trap a17 through the branch gas path a5 and the six-way membrane valve a16, the target compound is re-adsorbed by the secondary cold trap a17, the carrier gas is discharged through the flow path selection switch valve B19 and the flow controller B20, and then S2 is repeated.
S4, introducing the target compound carried by the carrier gas into a secondary cold trap device B3 through a branch gas circuit B6 to adsorb the target compound, and simultaneously operating the step S2 to release the target compound in the primary desorption device 1 again, wherein the specific steps are as follows:
as shown in fig. 5, the six-way membrane valve B21 and the flow path selection switch valve C24 are opened, the carrier gas carrying the target compound in the gas path 4 enters the secondary cold trap B22 through the branch gas path B6 and the six-way membrane valve B21, the target compound is re-adsorbed by the secondary cold trap B22, the carrier gas is discharged through the flow path selection switch valve C24 and the flow controller C25, and then S2 is repeated.
S5, dry blowing is carried out on the secondary cold trap device A2 and the secondary cold trap device B3, and the specific steps are as follows:
as shown in fig. 6, the carrier gas switch valve A8, the flow path selection switch valve B19, and the flow path selection switch valve C24 are opened, the dried carrier gas is introduced into the gas path 4 through the carrier gas pressure detector 9, the precision pressure regulating valve 10, and the carrier gas switch valve A8, and is shunted through the branch gas path a5 and the branch gas path B6 to enter the secondary cold trap a17 and the secondary cold trap B22, so as to carry the moisture in the secondary cold trap a17 and the secondary cold trap B22, the carrier gas carrying the moisture in the secondary cold trap a17 is discharged through the flow path selection switch valve B19 and the flow controller B20, and the carrier gas carrying the moisture in the secondary cold trap B22 is discharged through the flow path selection switch valve C24 and the flow controller C25.
S6, desorbing the target compounds in the secondary cold trap device A2 and the secondary cold trap device B3, and simultaneously introducing the target compounds into two analysis pipelines of a chromatograph for analysis and determination, wherein the method specifically comprises the following steps:
as shown in fig. 7, the six-way membrane valve a16 is opened, the carrier gas enters the secondary cold trap a17 through the carrier gas inlet a18, the carrier gas carries the target compound in the secondary cold trap a17 into the chromatograph for analysis and measurement, the six-way membrane valve B21 is opened, the carrier gas enters the secondary cold trap B22 through the carrier gas inlet B23, and the carrier gas carries the target compound in the secondary cold trap B22 into the chromatograph for analysis and measurement.
Example 2: a method for a dual-channel thermal desorption sampling system for chromatograph detection comprises the following steps:
s1, carrying out dry blowing on a primary desorption device 1, which comprises the following specific steps:
as shown in fig. 8, the carrier gas switch valve B12 and the flow path selection switch valve a14 are opened, the carrier gas is introduced into the primary desorption pipe 11 through the carrier gas switch valve B12, the dried carrier gas reversely purges the primary desorption pipe 11 to carry out moisture in the primary desorption pipe 11, and the flow controller a15 controls the flow rate of the primary dry blowing.
S2, releasing the target compound in the first-stage desorption device 1, which comprises the following specific steps:
as shown in fig. 9, the first-stage desorption/transfer membrane valve 7 and the carrier gas switch valve A8 are opened, the first-stage desorption/transfer tube 11 is heated to release the target compound adsorbed in the first-stage desorption/transfer tube 11, the carrier gas enters the first-stage desorption/transfer tube 11 through the precision pressure regulating valve 10, the carrier gas pressure detector 9 and the carrier gas switch valve A8, and the released target compound is carried into the gas path 4.
S3, the carrier gas carries the target compound and is respectively introduced into a second-stage cold trap device A2 and a second-stage cold trap device B3 through a branch gas circuit A5 and a branch gas circuit B6, and the target compound is adsorbed by the second-stage cold trap device A2 and the second-stage cold trap device B3, which are as follows:
as shown in fig. 10, the six-way membrane valve a16 and the flow path selection switch valve B19 are opened, the carrier gas carrying the target compound in the gas path 4 is diverted, part of the carrier gas enters the secondary cold trap a17 through the branch gas path a5 and the six-way membrane valve a16, the target compound is re-adsorbed by the secondary cold trap a17, and the carrier gas is discharged through the flow path selection switch valve B19 and the flow controller B20;
meanwhile, a six-way membrane valve B21 and a flow path selection switch valve C24 are opened, carrier gas carrying the target compound in the gas path 4 is shunted, part of the carrier gas enters a secondary cold trap B22 through a branch gas path B6 and the six-way membrane valve B21, the target compound is re-adsorbed by the secondary cold trap B22, and the carrier gas is discharged through the flow path selection switch valve C24 and a flow controller C25;
the carrier gas diverted from branch gas circuit a5 and branch gas circuit B6 may be diverted equally or unequally depending on the analysis.
S4, dry blowing is carried out on the secondary cold trap device A2 and the secondary cold trap device B3, and the specific steps are as follows:
as shown in fig. 11, the carrier gas switch valve A8, the flow path selection switch valve B19, and the flow path selection switch valve C24 are opened, the dried carrier gas is introduced into the gas path 4 through the carrier gas pressure detector 9, the precision pressure regulating valve 10, and the carrier gas switch valve A8, and is shunted through the branch gas path a5 and the branch gas path B6 to enter the secondary cold trap a17 and the secondary cold trap B22, so as to carry the moisture in the secondary cold trap a17 and the secondary cold trap B22, the carrier gas carrying the moisture in the secondary cold trap a17 is discharged through the flow path selection switch valve B19 and the flow controller B20, and the carrier gas carrying the moisture in the secondary cold trap B22 is discharged through the flow path selection switch valve C24 and the flow controller C25.
S5, desorbing the target compounds in the secondary cold trap device A2 and the secondary cold trap device B3, and simultaneously introducing the target compounds into two analysis pipelines of a chromatograph for analysis and determination, wherein the method specifically comprises the following steps:
as shown in fig. 12, the six-way membrane valve a16 is opened, the carrier gas enters the secondary cold trap a17 through the carrier gas inlet a18, the carrier gas carries the target compound in the secondary cold trap a17 into the chromatograph for analysis and measurement, the six-way membrane valve B21 is opened, the carrier gas enters the secondary cold trap B22 through the carrier gas inlet B23, and the carrier gas carries the target compound in the secondary cold trap B22 into the chromatograph for analysis and measurement.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, 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.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The utility model provides a binary channels thermal desorption sampling system for chromatograph detects which characterized in that: including one-level desorption device (1), second grade cold trap device A (2), second grade cold trap device B (3), one-level desorption device (1) output is provided with gas circuit (4), gas circuit (4) reposition of redundant personnel is branch road gas circuit A (5) and branch road gas circuit B (6), the input of second grade cold trap device A (2) is connected in branch road gas circuit A (5), the input of second grade cold trap device B (3) is connected in branch road gas circuit B (6), the chromatograph is all connected to the output of second grade cold trap device A (2) and second grade cold trap device B (3).
2. The dual-channel thermal desorption sampling system for chromatograph detection according to claim 1, wherein: one-level desorption device (1) includes that one-level desorption shifts membrane valve (7), carrier gas ooff valve A (8), carrier gas pressure detector (9), accurate pressure regulating valve (10), one-level desorption straw (11), the fourth end that one-level desorption shifted membrane valve (7) has carrier gas ooff valve A (8) through the tube coupling, the one end that one-level desorption shifted membrane valve (7) was kept away from in carrier gas ooff valve A (8) has carrier gas pressure detector (9) through the tube coupling, the one end that carrier gas ooff valve A (8) was kept away from in carrier gas pressure detector (9) has accurate pressure regulating valve (10) through the tube coupling, there is one-level desorption straw (11) through the tube coupling between the third end and the sixth end of one-level desorption shift membrane valve (7), gas circuit (4) is connected to the fifth end of one-level desorption shift membrane valve (.
3. The dual-channel thermal desorption sampling system for chromatograph detection according to claim 2, wherein: carrier gas pressure detector (9) still connect carrier gas ooff valve B (12) through the pipeline, carrier gas ooff valve B (12) are through the first end of tube coupling one-level desorption transfer membrane valve (7), the second end that one-level desorption transferred membrane valve (7) is connected with leak detection pressure detector (13) through the pipeline, the one end that one-level desorption was kept away from in leak detection pressure detector (13) is connected with flow path selection switch valve A (14) through the pipeline, the one end that leak detection pressure detector (13) were kept away from in flow path selection switch valve A (14) is connected with flow controller A (15) through the pipeline.
4. The dual-channel thermal desorption sampling system for chromatograph detection according to claim 1, wherein: second grade cold trap device A (2) are including six-way membrane valve A (16), second grade cold trap A (17), flow path selection switch valve B (19), flow controller B (20), branch circuit gas circuit A (5) are connected to the first end of six-way membrane valve A (16), there is second grade cold trap A (17) through the tube coupling between the third end of six-way membrane valve A (16) and the sixth end, there is flow path selection switch valve B (19) through the tube coupling to the second end of six-way membrane valve A (16), there is flow controller B (20) through the tube coupling to the one end that flow path selection switch valve B (19) kept away from six-way membrane valve A (16).
5. The dual-channel thermal desorption sampling system for chromatograph detection according to claim 4, wherein: the fourth end of the six-way membrane valve A (16) is connected with a carrier gas inlet A (18), and the fifth end of the six-way membrane valve A (16) is connected with a chromatograph.
6. The dual-channel thermal desorption sampling system for chromatograph detection according to claim 1, wherein: second grade cold trap device B (3) are including six-way membrane valve B (21), second grade cold trap B (22), flow path selection switch valve C (24), flow controller C (25), branch circuit gas circuit B (6) are connected to the first end of six-way membrane valve B (21), there is second grade cold trap B (22) through the tube coupling between the third end of six-way membrane valve B (21) and the sixth end, there is flow path selection switch valve C (24) through the tube coupling to the second end of six-way membrane valve B (21), there is flow path selection switch valve C (25) through the tube coupling to the one end that six-way membrane valve B (21) was kept away from to flow path selection switch valve C (24).
7. The dual-channel thermal desorption sampling system for chromatograph detection according to claim 6, wherein: the fourth end of the six-way membrane valve B (21) is connected with a carrier gas inlet passage B (23), and the fifth end of the six-way membrane valve B (21) is connected with a chromatograph.
8. The dual-channel thermal desorption sampling system for chromatograph detection according to claim 1, wherein: the air passage (4), the branch air passage A (5) and the branch air passage B (6) are integrally formed.
9. The method of claim 1 for the dual channel thermal desorption sampling system for chromatograph detection, comprising the steps of:
s1, carrying out dry blowing on a primary desorption device (1);
s2, releasing the target compound in the first-stage desorption device (1);
s3, introducing the carrier gas carrying the target compound into a secondary cold trap device A (2) through a branch gas circuit A (5) to adsorb the target compound, and simultaneously operating the step S2 to release the target compound in the primary desorption device (1);
s4, introducing the carrier gas carrying the target compound into a secondary cold trap device B (3) through a branch gas circuit B (6) to adsorb the target compound, and simultaneously operating the step S2 to release the target compound in the primary desorption device (1) again;
s5, dry blowing is carried out on the secondary cold trap device A (2) and the secondary cold trap device B (3);
s6, desorbing the target compounds in the secondary cold trap device A (2) and the secondary cold trap device B (3), and simultaneously introducing the target compounds into two analysis pipelines of a chromatograph for analysis and determination.
10. The method of claim 1 for the dual channel thermal desorption sampling system for chromatograph detection, comprising the steps of:
s1, carrying out dry blowing on a primary desorption device (1);
s2, releasing the target compound in the first-stage desorption device (1);
s3, introducing the carrier gas carrying the target compound into a secondary cold trap device A (2) and a secondary cold trap device B (3) through a branch gas circuit A (5) and a branch gas circuit B (6) respectively, and adsorbing the target compound by the secondary cold trap device A (2) and the secondary cold trap device B (3);
s4, dry blowing is carried out on the secondary cold trap device A (2) and the secondary cold trap device B (3);
and S5, desorbing the target compounds in the secondary cold trap device A (2) and the secondary cold trap device B (3), and simultaneously introducing the target compounds into two analysis pipelines of a chromatograph for analysis and determination.
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