CN117871702A - Gas chromatography rapid analysis device and method - Google Patents

Abstract

The invention discloses a gas chromatography analysis device and a method, and relates to the technical field of gas analysis and application, wherein the device comprises a plurality of groups of parallel sample injection separation loops, and the sample injection separation loops are connected with a detector and a data analysis and control system; each sample injection separation loop comprises a sample airflow pipeline, a flow path switching valve, a gas diaphragm pump and a ten-way valve which are connected in sequence; the gas diaphragm pump, the gas quantitative ring, the chromatographic separation column, the carrier gas pipeline, the electromagnetic valve and the check valve are respectively connected with different interfaces of the ten-way valve, and the check valve is connected with the detector. The separation of the interference component and the target component is realized through a chromatographic separation column, and the independent detection of the target component is realized through reasonably switching the interval time of the separation column connected with a detector; continuous detection of the target component is realized by reasonably switching the interval time of the separation column in each loop to the detector. The device and the method provided by the invention can greatly shorten the detection period of a single sample and realize the online real-time analysis of the gas.

Description

Gas chromatography rapid analysis device and method

Technical Field

The invention belongs to the technical field of gas analysis and application, and particularly relates to a gas chromatography rapid analysis device and method.

Background

The main control room of the nuclear power plant is a central center for controlling the overall state of the nuclear power plant, plays the main functions of ensuring the safe operation of the unit, improving the availability of the unit, ensuring the safety of equipment and personnel, and the like, and plays an important role in controlling the further diffusion of dangers and reducing the hazard of accidents under the accident working condition. In order to ensure the usability of the main control room under accident working conditions, a tracer is generally adopted to detect the air leakage in the main control room without filtering. The trace gas is selected to meet the requirements of no toxicity, nonflammability, inert gas, extremely low background concentration in air, measurable extremely low concentration, difficult absorption by various materials, no release of such gases by the materials existing in the main control room, and the like. Sulfur hexafluoride (SF) ₆ ) The gas has stable chemical property, is nontoxic and not easy to adsorb, and is local to the master control roomThe concentration is extremely low. Therefore, the main control room is free from filtered air internal leakage detection, and sulfur hexafluoride is usually adopted as trace gas for analysis and detection.

The method for detecting the concentration of sulfur hexafluoride in the air generally comprises the following steps: techniques and methods such as gas chromatography, infrared absorption spectroscopy, photoacoustic spectroscopy, and laser remote detection, wherein infrared absorption spectroscopy and photoacoustic spectroscopy have a fast detection rate, but have low detection accuracy; the gas chromatography and the laser remote detection method have higher detection precision, but the single sample detection period is longer, and the real-time detection cannot be performed, so that the injection of the tracer gas and the balance of the concentration of the tracer gas in the test process are guided. In the master control room leakage test, the collected sample gas is mixed gas of sulfur hexafluoride trace gas and air, and the sample peak spectrum in the gas chromatography analysis process has corresponding characteristic peak spectrums shown by other gas components including oxygen and the like besides the characteristic peak spectrum of the target gas sulfur hexafluoride. The characteristic peak spectrum of other gas components is useless and may interfere with the sulfur hexafluoride gas peak spectrum. In general, the type and length of chromatographic column are selected according to the physical characteristics of the interference component in the mixed gas, and in addition, in the aspect of detection process, proper carrier gas type, carrier gas flow rate, gas separation, detection temperature and other process parameters are selected to realize effective separation of the target component gas (sulfur hexafluoride) and the interference component gas, so that accurate quantitative measurement of the target gas is realized through the corresponding relation between the peak spectrum characteristics (peak height, peak area and the like) of the target gas and the calibration curve in the corresponding detector measurement spectrogram. The separation and detection process of the gas component and the target gas are disturbed, and the whole process takes 5-8 minutes. Wherein, the separation of the interfering component and the target gas in the chromatographic column accounts for the majority of the total time of sample detection. In addition, in general, gas chromatography is performed in an off-line analysis mode, and besides the time required for an analysis flow (carrier gas carrying sample gas sample injection, separation of component gases in a chromatographic column, detection of component gases in a detector and result recording), the time is also required for sample analysis interval, so that the analysis duration of a single sample is long. In the leakage test of the gas sample in the main control room of the constant concentration method, the concentration of the tracer in different areas of the main control room cannot be measured in real time, the concentration of the tracer in each area cannot be fed back in real time and guided to be quantitatively and rapidly supplemented and injected into the tracer injection equipment to carry out concentration adjustment, and the rapid balance of the concentration of the tracer in different areas of the main control room in the internal leakage measurement process cannot be realized. Real-time analysis of gas samples in different areas of the main control room is a key factor for limiting the technology of detecting the leakage in the main control by a constant concentration method.

Disclosure of Invention

Aiming at the defects in the prior art, the invention aims to provide a gas chromatography rapid analysis device and a gas chromatography rapid analysis method, and the device and the method can greatly shorten the detection period of single sample gas, improve the sample analysis efficiency and realize the online real-time analysis of trace gas.

In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:

a gas chromatograph rapid analysis device, the device comprising: the sample injection separation loop is connected with a detector, and the detector is connected with the data analysis and control system;

the sample injection separation loops are arranged in a parallel mode, and the sample injection separation loops are connected with the detector and the data analysis and control system;

each sample injection separation loop comprises a sample airflow pipeline, a flow path switching valve connected with the sample airflow pipeline, a gas diaphragm pump connected with the flow path switching valve and a ten-way valve; the ten-way valve comprises ten interfaces, the gas diaphragm pump, the gas quantitative ring, the chromatographic separation column, the carrier gas pipeline, the electromagnetic valve and the one-way valve are respectively connected with different interfaces of the ten-way valve, and the one-way valve is connected with the detector; the data analysis and control system is respectively connected with the flow path switching valve, the gas diaphragm pump, the ten-way valve, the carrier gas pipeline, the electromagnetic valve and the detector through logic control signals;

the gas flow pipeline is used for providing sample gas to be detected, the sample gas to be detected, which is correspondingly connected with the gas flow pipeline, is injected into the gas quantitative ring through the flow path switching valve, and the gas quantitative ring passes through the chromatographic separation column with a fixed volume to separate the interference gas component from the target gas component in the sample gas; detecting a target gas component by the detector; and the data analysis and control system controls the switching of the valve of the ten-way valve to realize the on-off of different flow paths.

Further, in the gas chromatography rapid analysis device, the gas flow pipeline is connected with the flow path switching valve in a mode of multiple groups of gas flow pipelines arranged in parallel.

Further, the gas chromatography rapid analysis device has the advantages that the gas diaphragm pump has two working modes of continuous operation and timed intermittent operation.

Further, in the gas chromatography rapid analysis device, the gas diaphragm pump is connected with the fourth interface of the ten-way valve; two ends of the gas quantitative ring are respectively connected with a second interface and a fifth interface of the ten-way valve; the airflow inlet and the airflow outlet of the chromatographic separation column are respectively connected with a sixth interface and a ninth interface of the ten-way valve; the one-way valve is connected with an eighth interface of the ten-way valve; and the third port and the tenth port of the ten-way valve are connected with an exhaust pipe to directly exhaust the waste gas or discharge the waste gas to a specified collection container.

Further, as described above, the gas chromatography rapid analysis device, the carrier gas pipeline includes a first carrier gas pipeline and a second carrier gas pipeline that are arranged in parallel, the second carrier gas pipeline and the first carrier gas pipeline are respectively connected with the first interface and the seventh interface of the ten-way valve, and the electromagnetic valve is disposed between the first carrier gas pipeline and the seventh interface of the ten-way valve.

Further, in the gas chromatograph rapid analysis device as described above, the carrier gas in the first carrier gas pipeline and the second carrier gas pipeline is high-purity gas with set flow, and different flow rates are set by the data analysis and control system at different stages of the carrier belt.

Further, according to the gas chromatography rapid analysis device, the data analysis and control system is used for controlling the flow path switching valve to connect different sample gases according to the gas detection setting requirement, controlling the timing start and stop of the gas diaphragm pump, controlling the periodic switching of the ten-way valve, controlling the setting of carrier gas flow, controlling the on-off of the electromagnetic valve, and analyzing, calculating and outputting detection data of the detector.

A method for performing gas chromatography rapid analysis based on the gas chromatography rapid analysis device described above, comprising the following:

s1, separating an interference gas component from a target gas component in sample gas through a chromatographic separation column, and reasonably switching the interval time of the chromatographic separation column when the chromatographic separation column is connected into a detection loop, so that the independent detection of the target gas component is realized;

s2, reasonably switching the interval time of the chromatographic separation column in each path of sample introduction separation loop to the detection loop by arranging the multipath sample introduction separation loops in parallel, thereby realizing continuous detection of the target gas component.

Further, in the gas chromatography rapid analysis method as described above, for a single sample injection separation loop, step S1 is specifically:

s11, disconnecting the chromatographic separation column from the detector, and evacuating and removing substances before the peak of the target gas component through the chromatographic separation column;

s12, when the target gas component in the chromatographic separation column is about to flow out of the chromatographic separation column, the chromatographic separation column is connected into a detector, and the target gas component is detected in the detector;

s13, disconnecting the chromatographic separation column from the detector again after the complete target gas component spectrum peak is completed, so that the target gas component is detected independently.

Further, in the gas chromatography rapid analysis method as described above, for the plurality of sample injection separation circuits arranged in parallel, step S2 specifically includes:

s21, after all target gas components in the first sample injection separation loop enter the detector, switching the current separation column loop to a parallel second sample injection separation loop according to a set time interval, and ensuring that the gas components before the target gas components in the second sample injection separation loop are just discharged through reasonable process parameter setting, wherein the target gas components in the second sample injection separation loop enter the detector for analysis and detection after a shorter time interval;

s22, sequentially sending the target gas components separated in each sample injection separation loop into a detector for analysis and detection according to the method of the step S21, so as to realize continuous detection of the target gas components.

Compared with the prior art, the gas chromatography rapid analysis device and method provided by the invention have the following beneficial effects:

according to the invention, through automatic sample gas injection (carrier gas is injected into the chromatographic column under the carrier), parallel and sequential separation of a plurality of groups of sample gas in the corresponding chromatographic column (separation of target gas and interference component gas), sequential entry of the target component gas after removal of the interference component into the detector according to a set interval time for rapid continuous detection analysis (only the target component gas enters the detector), and continuous cyclic detection under program control, rapid and accurate detection analysis of the target component in the sample gas is realized.

Drawings

Fig. 1 is a schematic structural diagram of a gas chromatograph rapid analysis device according to an embodiment of the present invention;

FIG. 2 is a flow chart of a gas chromatography rapid analysis method provided in an embodiment of the invention;

FIG. 3 is a diagram showing the analysis of sulfur hexafluoride gas chromatography in air obtained by conventional methods under certain conditions of determining the detection parameters;

FIG. 4 is a diagram of a chromatographic analysis of sulfur hexafluoride obtained when a gas sample is detected using the method provided by the invention under the same conditions of detection parameters as those of FIG. 3;

in the figure: 1-gas flow pipeline, 2-flow path switching valve, 3-gas diaphragm pump, 4-gas quantitative ring, 5-ten-way valve, 6-chromatographic separation column, 7-carrier gas pipeline, 8-electromagnetic valve, 9-one-way valve, 10-detector, 11-data analysis and control system; 501-first interface, 502-second interface, 503-third interface, 504-fourth interface, 505-fifth interface, 506-sixth interface, 507-seventh interface, 508-eighth interface, 509-ninth interface, 510-tenth interface, 701-first carrier gas line, 702-second carrier gas line.

Detailed Description

The invention is described in further detail below with reference to the drawings and the detailed description.

Fig. 1 shows a schematic structural diagram of a gas chromatography rapid analysis device according to an embodiment of the present invention, where the device includes a sample separation circuit, and the sample separation circuit is connected to a detector 10, and the detector 10 is connected to a data analysis and control system 11. The sample injection separation loop is arranged in a parallel mode by adopting a plurality of groups of sample injection separation loops according to the detected gas separation and detection requirements, and the plurality of groups of sample injection separation loops are commonly connected with a detector 10 and a data analysis and control system 11; each sample injection separation loop comprises a sample airflow pipeline 1, a flow path switching valve 2, a gas diaphragm pump 3, a gas quantitative ring 4, a ten-way valve 5, a chromatographic separation column 6, a carrier gas pipeline 7, an electromagnetic valve 8 and a one-way valve 9, wherein the airflow pipeline 1 is connected with the flow path switching valve 2 in a mode of a plurality of groups of parallel arrangement, the flow path switching valve 2 is connected with the ten-way valve 5 through the gas diaphragm pump 3, and required detection gas connected with the corresponding airflow pipeline 1 is injected into the gas quantitative ring 4 connected with the ten-way valve 5 through the flow path switching valve 2; the ten-way valve 5 comprises ten interfaces, the gas quantitative ring 4, the chromatographic separation column 6, the carrier gas pipeline 7 and the one-way valve 9 are respectively connected with different interfaces of the ten-way valve 5, the one-way valve 9 is connected with the detector 10, and the switching of the valve of the ten-way valve 5 is controlled by the data analysis and control system 11 according to the detection setting requirement to realize the on-off of different flow paths.

The air flow pipeline 1 can be connected with a container and a device for collecting sample gas, such as a gas sampling bag, or can be directly arranged at a specific position of a sample to be collected in a branch pipe mode through a pipe network, for example, when a leak detection test is performed in a main control room, the air flow pipeline 1 is arranged at a representative position of different areas of the main control room to collect a representative gas sample.

The flow path switching valve 2 is used for conveying the sample gas in the corresponding positions of different branch pipes of the gas flow pipeline 1 or the container to the gas quantifying ring 4 under the control of the data analysis and control system 11 according to the detection requirement of the sample gas.

The gas diaphragm pump 3 has two working modes, and can perform continuous operation sampling or timed intermittent operation sampling under the control of the data analysis and control system 11 according to the requirements. For example, when the gas flow pipeline 1 is connected with the target sampling position, the gas diaphragm pump 3 can continuously operate to collect sample gas; when the air flow pipeline 1 is connected with a sample container such as a sampling bag, the air diaphragm pump 3 can be matched with the flow path switching valve 2 and the ten-way valve 5 to perform intermittent operation and sampling at fixed time according to specific set requirements.

The gas dosing ring 4 is used to fix the sample gas volume to a certain value, ensuring that the sample gas volume is consistent each time. Depending on the physical properties, concentration and other detection requirements of the detected gas, quantitative rings with different volume capacities and different materials, such as 1ml, 2ml and the like, stainless steel pipes, glass pipes and the like, can be adopted.

The carrier gas line 7 is a carrier gas flow line, and includes a first carrier gas line 701 and a second carrier gas line 702 arranged in parallel, and the ports to which the ten-way valve 5 and the second carrier gas line 702 are connected are defined as a first port 501, and the other ports are numbered in a counterclockwise order. The method comprises the following steps: the second carrier gas pipeline 702 and the first carrier gas pipeline 701 are respectively connected with the first interface 501 and the seventh interface 507 of the ten-way valve, the diaphragm pump 3 is connected with the fourth interface 504 of the ten-way valve, two ends of the gas quantitative ring 4 are respectively connected with the second interface 502 and the fifth interface 505 of the ten-way valve, the gas flow inlet and the gas flow outlet of the chromatographic column 6 are respectively connected with the sixth interface 506 and the ninth interface 509 of the ten-way valve, the eighth interface 508 of the ten-way valve is connected with the one-way valve 9, the third interface 503 and the tenth interface 510 of the ten-way valve are connected with the exhaust pipe, and the waste gas is directly exhausted or discharged to a specified collecting container. According to the detection setting requirements, the data analysis and control system 11 controls the switching of the valve of the ten-way valve 5 to realize the on-off of different flow paths.

The chromatographic separation column 6 is used for separation of the interfering gas components from the target gas components in the sample gas. In the gas two-phase motion, the translation speed of the different component gases along the chromatographic separation column 6 is different, and the separation of the different component gases is realized by utilizing the speed difference. The chromatographic separation column 6 with different types, lengths and pipe diameters is selected according to the composition type, physical property, concentration and other detection requirements of the analyzed gas.

The carrier gas flows into the ten-way valve 5 from the carrier gas pipeline 7, and can be different types of sample carrier gases such as high-purity nitrogen, hydrogen and the like according to the analyzed target gas and the corresponding detector. The first carrier gas pipeline 701 is internally provided with an electromagnetic valve 8, and the opening or closing of the electromagnetic valve 8 is controlled by a data analysis and control system 11 according to the gas analysis and detection requirements to realize the on-off of the first carrier gas pipeline 701; the second carrier gas line 702 may continue to supply gas to the ten-way valve 5. The carrier gas in the first carrier gas pipeline 701 and the second carrier gas pipeline 702 is high-purity gas with set flow rate, and different flow rates/flow rates are set by the data analysis and control system 11 at different stages of the carrier belt (for example, the residual gas components of the chromatographic column after the target gas comes out of the peak can be quickly purged and eluted by adopting high-flow carrier gas).

The check valve 9 is connected to the detector 10 for ensuring that the air flow in the flow path flows in a single direction to the detector 10. The target component gas flowing out of the ten-way valves 5 in each sample-taking separation loop arranged in parallel is sequentially conveyed to the detector 10 for analysis and measurement at reasonable intervals under the control of the data analysis and control system 11. The ECD detector is used for sulfur hexafluoride gas analysis, and other types of detectors such as a thermal conductivity detector, a flame ionization detector, a flame luminosity detector and other types of gas chromatographic analysis detection can be corresponding to other types of detectors when other target gas analysis is performed.

The data analysis and control system 11 is connected with the flow path switching valve 2, the gas diaphragm pump 3, the ten-way valve 5, the carrier gas pipeline 7, the electromagnetic valve 8 and the detector 10 through logic control signals respectively. The data analysis and control system 11 is used for controlling the flow path switching valve 2 to connect different sample gases according to the gas detection setting requirement, controlling the timing start and stop of the gas diaphragm pump 3, controlling the periodic switching of the ten-way valve 5, controlling the setting of the carrier gas flow, controlling the on-off of the electromagnetic valve 8, and analyzing, calculating and outputting the detection data of the detector 10.

In the invention, two detectors (two detectors are arranged on one gas chromatograph) can be arranged in parallel, and the number of corresponding parallel sample injection separation loops is doubled, so that the analysis period is further shortened, and the detection efficiency is improved.

The working principle and the process of the device are as follows: the gas chromatography uses the principle of chromatographic separation analysis, and in the gas two-phase motion, the separation of different component gases is realized through the difference of the translation speed of the different component gases along a chromatographic column, and the different component gases finish signal conversion in a detector of the gas chromatograph in sequence, so that the gas concentration is converted into a detectable electric signal.

The analysis chart of the sulfur hexafluoride gas chromatography in the air under the condition of certain detection parameters is shown in fig. 2, an oxygen peak appears near 1.8min, and the sulfur hexafluoride peak position is near 3.9 min. By adopting a traditional chromatographic analysis flow, sulfur hexafluoride gas is analyzed from sample injection to completion, one analysis period is about 5-8min, twelve samples are analyzed in one hour at most, and the analysis and detection rate is low.

The invention provides a gas chromatography rapid analysis method based on the device, which comprises the following core contents:

s1, separating an interference gas component from a target gas component by arranging a chromatographic separation column, and realizing independent detection of the target gas component by reasonably switching the interval time of the chromatographic separation column when the chromatographic separation column is connected into a detection loop;

s2, reasonably switching the interval time of each chromatographic separation column connected to the detection loop by arranging a plurality of chromatographic separation columns in parallel, thereby realizing continuous detection of the target gas component.

For single detection, disconnecting the chromatographic separation column from the detector, and evacuating and removing substances before the peak of the target gas component through the chromatographic separation column; when the target gas component in the chromatographic separation column is about to flow out of the chromatographic separation column, the chromatographic separation column is connected into a detector, and the target gas component is detected in the detector; after the complete peak of the target gas component spectrum is completed (all target gas components enter the detector), the separation column is disconnected from the chromatographic detector again. The target gas component is separated through the chromatographic separation column, and the independent detection of the target gas component is realized by reasonably switching the interval time of the chromatographic separation column accessing the detection loop. And after the chromatographic separation column is disconnected with the detector, all the other components of the sample gas in the separation column are purged and eluted under the purging of the carrier gas, so that one-time detection is completed.

In continuous detection, through parallel multichannel chromatographic separation columns, the interval time of each chromatographic separation column access detection loop is reasonably switched, thereby realizing the high-efficiency utilization of a detection instrument. The parallel separation technology of the multi-path chromatographic separation column is matched with gas automatic sample injection, so that uninterrupted detection of target components can be realized, the detection rate of the target gas components is improved, and the online real-time analysis is ensured.

The realization of rapid detection of sample gas by interfering component gas separation is a key of real-time detection and analysis of target component gas. The invention adopts a mode of arranging a chromatographic separation column to sequentially separate different components of sample gas passing through the separation column, and the time of flowing out of the chromatographic separation column through each component gas is different, and the separated component gas before the target gas component is directly emptied and then the chromatographic separation column is connected to a detector for detecting and analyzing the concentration of the target gas. After all target gas components enter the detector, the current separation column loop is switched to a parallel second separation loop according to a set time interval (2-5 seconds), the gas components just before the target gas components in the next separation loop are discharged through reasonable process parameter setting, and the target gas components in the second separation loop enter the detection loop for analysis and detection after a shorter time interval (2-5 seconds). Similarly, the parallel pre-separation loops sequentially send the separated target gas components into the detection loop for analysis and detection, and the detector continuously detects the target gas components in the next sample at shorter time intervals (2-5 seconds) after completing a complete detection period (for example, 20-25 seconds) of the target gas components, so that the detection and analysis time of a single sample is greatly shortened. To ensure consistent sample gas volumes each time, the present invention uses a dosing ring to fix the sample gas volumes to a defined value.

The sulfur hexafluoride chromatogram when the device and the method provided by the invention are used for detecting the gas sample is shown in figure 4.

The parallel separation circuits of the invention can be corresponding to one detector, and also can be corresponding to two parallel detectors. When the detection device is a single detector, the single sample detection period is the necessary detection time of the pure sulfur hexafluoride component, the loop switching time, the redundancy time for eliminating the baseline disturbance generated by valve switching, the redundancy time reserved for prolonging the separation time of the target gas component which possibly occurs in the separation column after the measurement of a large number of samples and other process redundancy time. When the detection device is a double detector, the corresponding separation loop is doubled, and the detection period of a single sample is shortened to be half of that of a single detector.

Examples

The method steps for rapidly analyzing sulfur hexafluoride tracer gas by using the gas chromatography rapid analysis device provided by the invention are described in detail below.

Step one, cleaning and inflating a gas quantitative ring. The ten-way valve 5 is set to be in a state of inflating the gas dosing ring 4 by the data analysis and control system 11, specifically: the flow path switching valve 2 charges the gas quantifying ring 4 with the required detection target sample gas through the corresponding gas flow pipeline 1, and the quantifying ring is cleaned and filled with the gas to be analyzed through continuous charging for a set time. The connection of the inflation flow path is as follows: the gas flow pipeline 1, the flow path switching valve 2, the gas diaphragm pump 3, the tenth-way valve fourth interface 501, the tenth-way valve fifth interface 505, the gas dosing ring 4, the tenth-way valve second interface 502, the tenth-way valve third interface 503 and the exhaust pipeline.

The second carrier gas line 702 is evacuated through the ten way valve 5, the flow path connection being: a second carrier gas line 702, a ten-way valve first port 501, a ten-way valve tenth port 510, and an exhaust line.

The first carrier gas line 701 is closed by the solenoid valve 8, and the flow path is interrupted. The physical connection sequence is as follows: a first carrier gas line 701, a solenoid valve 8, a tenth port 507, a tenth port 506, a chromatographic separation device, a tenth port 509, a tenth port 508, a check valve 9, and an ECD detector 10.

And step two, separating each component gas of the sample gas in the chromatographic separation column and evacuating the gas sample before the target component gas such as sulfur hexafluoride flows out of the separation column. The method comprises the following steps: after the first step is completed, the data analysis and control system 11 controls the ten-way valve 5 to switch the valve. The sampling airflow flow path after valve switching is as follows: the gas flow pipeline 1, the flow path switching valve 2, the gas diaphragm pump 3, the tenth-way valve fourth interface 504, the tenth-way valve third interface 503 and the exhaust pipeline. The sample gas at the next analysis position is emptied through the flow path switching valve 2, and the process is used for cleaning the whole flow path to ensure that the target gas concentration at each part of the whole flow path is consistent with the concentration at the sampling site.

The second carrier gas line 702 carries the sample gas in the dosing ring through the ten-way valve 5 into the separation column for separation and evacuates all the gas before the target component gas. The flow path connection is: the second carrier gas pipeline 702, the first port 501 of the ten-way valve, the second port 502 of the ten-way valve, the dosing ring, the fifth port 505 of the ten-way valve, the sixth port 506 of the ten-way valve, the separation column, the ninth port 509 of the ten-way valve, the tenth port 510 of the ten-way valve and the exhaust pipeline.

The second carrier gas line 702 is closed by the solenoid valve 8, and the flow path is interrupted. The physical connection sequence is as follows: a first carrier gas line 701, a solenoid valve 8, a tenth valve seventh port 507, a tenth valve eighth port 508, a check valve 9, and an ECD detector 10.

And thirdly, detecting and analyzing the target component gas and inflating a ring with a given amount of gas at the next analysis position. After the second procedure is completed, the data analysis and control system 11 controls the ten-way valve 5 to switch the valve. The ten-way valve 5 is set to be in an inflated state for the gas dosing ring 4 by the data analysis and control system 11, and a similar procedure is performed. The method comprises the following steps: and (3) inflating the gas quantifying ring 4 with the detection target gas required for cleaning the whole flow path in the second step, and cleaning and filling the quantifying ring with the gas to be analyzed through continuous inflation for a set time. The connection of the inflation flow path is as follows: the gas flow pipeline 1, the flow path switching valve 2, the gas diaphragm pump 3, the tenth-way valve fourth interface 504, the tenth-way valve fifth interface 505, the gas dosing ring 4, the tenth-way valve second interface 502, the tenth-way valve third interface 503 and the exhaust pipeline.

The second carrier gas line 702 is evacuated through the ten way valve 5, the flow path connection being: a second carrier gas line 702, a ten-way valve first port 501, a ten-way valve tenth port 510, and an exhaust line.

The first carrier gas line 701 is opened by the solenoid valve 8, the flow path is connected to the detector, and the carrier gas feeds the target component gas to be discharged from the separation column to the detector for detection and analysis. The flow path connection sequence is as follows: a first carrier gas pipeline 701, a solenoid valve 8, a tenth port 507 of the tenth port 5-7, a tenth port 506 of the tenth port, a chromatographic separation device, a tenth port 509 of the tenth port, an eighth port 508 of the tenth port, a check valve 9 and an ECD detector 10.

And fourthly, purging and eluting residual component gas in the chromatographic column. If the target component gas is the last single gas separated by the chromatographic column or other component gases after the target component gas do not respond in the detector and do not generate detection peak spectrums, the first, second and third process steps are circulated to carry out analysis and detection of the target gas at the next required detection position. If the position of the target component gas in the gas is sufficiently back, or the residual component of the previous sample gas can be completely purged and eluted by the direct emptying process before the next sample gas pre-separation target component gas flows out, the first, second and third process steps are circulated to carry out the analysis and detection of the target gas at the next required detection position. If the other component gases remained in the separation column after the target component gas is completely discharged need a long time for purging and eluting to be completely discharged, a large flow carrier gas is needed for rapid and independent purging and eluting steps. The purging step is similar to the second step, and the second carrier gas line 702 purges and elutes the residual gas component in the separation column through the dosing ring. The flow path connection is: the second carrier gas pipeline 702, the first port 501 of the ten-way valve, the second port 502 of the ten-way valve, the dosing ring, the fifth port 505 of the ten-way valve, the sixth port 506 of the ten-way valve, the separation column, the ninth port 509 of the ten-way valve, the tenth port 510 of the ten-way valve and the exhaust pipeline.

The first carrier gas line 701 is closed by the solenoid valve 8, and the flow path is interrupted. The physical connection sequence is as follows: a first carrier gas line 701, a solenoid valve 8, a tenth valve seventh port 507, a tenth valve eighth port 508, a check valve 9, and an ECD detector 10.

Step five is similar to the above step one, step two, step three and step four, the parallel-arranged multi-way separation device carries the target component gas such as sulfur hexafluoride to the detector for analysis by a plurality of seconds (2-5 s) after the first ten-way valve first carrier gas pipeline 701 carries the next group of target component gas to the detector for analysis, for example, the second ten-way valve carrier gas carries the next group of target component gas to the detector for analysis by a plurality of seconds (2-5 s) after the second ten-way valve carrier gas carries the next group of target component gas to the detector for analysis, and the plurality of groups of parallel-arranged target component gas separation devices continuously circulate to the detector at fixed intervals to convey the separated target component gas, so that the circulation is realized, the detector achieves the maximum application, and the single sample analysis time is the shortest.

By adopting the analysis flow provided by the invention, the target component gas in the test sample is separated from other gases in advance by arranging the pre-separation chromatographic column. The outflow time of sulfur hexafluoride gas after passing through the chromatographic separation column is in the time period of t1 to t2 (proper redundant time is added before and after), the gas in the chromatographic separation column enters the chromatographic detector at the time t1 through flow path switching, and chromatographic sample injection lasts until the time t2, so that only the chromatographic peak of the target component gas is detected through chromatography, and the detection time is only or slightly more than the peak outlet time of the target component gas. In the chromatographic peak, taking sulfur hexafluoride as an example, the peak outlet time is about 20-25 s, other flow path switching time and moderate redundancy time are added, the conservation estimation of one sample analysis time is not more than 30-35 s, and 100-120 samples can be measured under the ideal working condition of matching with gas automatic sample injection per hour.

According to the gas chromatography rapid analysis device and method provided by the invention, substances before the peak of target gas are discharged and removed by arranging the chromatographic separation column, so that the separation of the interference gas component and the target gas component is realized; the separation column is reasonably switched to access the interval time of the detection loop so as to realize the independent detection of the target gas component; the parallel multi-path chromatographic separation columns are matched with gas automatic sample injection at the same time, and the interval time of each path of chromatographic separation column connected into the detection loop is reasonably switched, so that the high-efficiency utilization of the detection instrument is realized.

It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.

Claims (10)

1. A gas chromatograph rapid analysis device, the device comprising: the sample injection separation loop is connected with the detector (10), and the detector (10) is connected with the data analysis and control system (11);

the sample injection separation loops are arranged in a parallel mode, and the sample injection separation loops are connected with the detector (10) and the data analysis and control system (11) together;

each sample injection separation loop comprises a sample airflow pipeline (1), a flow path switching valve (2) connected with the sample airflow pipeline (1), a gas diaphragm pump (3) connected with the flow path switching valve (2) and a ten-way valve (5); the ten-way valve (5) comprises ten interfaces, the gas diaphragm pump (3), the gas quantitative ring (4), the chromatographic separation column (6), the carrier gas pipeline (7), the electromagnetic valve (8) and the one-way valve (9) are respectively connected with different interfaces of the ten-way valve (5), and the one-way valve (9) is connected with the detector (10); the data analysis and control system (11) is respectively connected with the flow path switching valve (2), the gas diaphragm pump (3), the ten-way valve (5), the carrier gas pipeline (7), the electromagnetic valve (8) and the detector (10) through logic control signals;

the gas flow pipeline (1) is used for providing sample gas to be detected, the gas flow pipeline (1) is correspondingly connected with the sample gas to be detected through the flow path switching valve (2) and is injected into the gas quantifying ring (4), and the gas quantifying ring (4) passes through the chromatographic separation column (6) through the sample gas with a fixed volume to separate the interference gas component from the target gas component in the sample gas; detecting a target gas component by means of the detector (10); and the data analysis and control system (11) is used for controlling the switching of the valve of the ten-way valve (5) to realize the on-off of different flow paths.

2. The rapid analysis device for gas chromatography according to claim 1, wherein the gas flow pipeline (1) is connected with the flow path switching valve (2) in a manner of a plurality of groups arranged in parallel.

3. The gas chromatography rapid analysis device according to claim 2, wherein the gas membrane pump (3) has two modes of operation, continuous operation and timed intermittent operation.

4. A gas chromatography rapid analysis device according to any one of claims 1-3, wherein the gas membrane pump (3) is connected to a fourth port (504) of the ten-way valve; two ends of the gas quantitative ring (4) are respectively connected with a second interface (502) and a fifth interface (505) of the ten-way valve; the gas flow inlet and the gas flow outlet of the chromatographic separation column (6) are respectively connected with a sixth interface (506) and a ninth interface (509) of the ten-way valve; the one-way valve (9) is connected with an eighth interface (508) of the ten-way valve; and a third interface (503) and a tenth interface (510) of the ten-way valve are connected with an exhaust pipe to directly exhaust or discharge the exhaust gas to a designated collection container.

5. The rapid gas chromatography device according to claim 4, wherein the carrier gas line (7) comprises a first carrier gas line (701) and a second carrier gas line (702) which are arranged in parallel, the second carrier gas line (702) and the first carrier gas line (701) are respectively connected with a first interface (501) and a seventh interface (507) of the ten-way valve, and the electromagnetic valve (8) is arranged between the first carrier gas line (701) and the seventh interface (507) of the ten-way valve.

6. The rapid gas chromatography device according to claim 5, wherein the carrier gas in the first carrier gas line (701) and the second carrier gas line (702) is a high purity gas with a set flow rate, and different flow rates/flow rates are set by the data analysis and control system (11) at different stages of the carrier tape.

7. The rapid analysis device for gas chromatography according to claim 1, wherein the data analysis and control system (11) is used for controlling the flow path switching valve (2) to connect different sample gases according to the gas detection setting requirement, controlling the timing start and stop of the gas diaphragm pump (3), controlling the periodical switching of the ten-way valve (5), controlling the setting of carrier gas flow, controlling the on-off of the electromagnetic valve (8), and analyzing, calculating and outputting the detection data of the detector (10).

8. A method of performing gas chromatography flash analysis using the gas chromatography flash analysis apparatus of any one of claims 1-7, comprising:

s1, separating an interference gas component from a target gas component in sample gas through a chromatographic separation column, and reasonably switching the interval time of the chromatographic separation column when the chromatographic separation column is connected into a detection loop, so that the independent detection of the target gas component is realized;

s2, reasonably switching the interval time of the chromatographic separation column in each path of sample introduction separation loop to the detection loop by arranging the multipath sample introduction separation loops in parallel, thereby realizing continuous detection of the target gas component.

9. The rapid analysis method according to claim 8, wherein for a single sample separation loop, step S1 is specifically:

s11, disconnecting the chromatographic separation column from the detector, and evacuating and removing substances before the peak of the target gas component through the chromatographic separation column;

s12, when the target gas component in the chromatographic separation column is about to flow out of the chromatographic separation column, the chromatographic separation column is connected into a detector, and the target gas component is detected in the detector;

s13, disconnecting the chromatographic separation column from the detector again after the complete target gas component spectrum peak is completed, so that the target gas component is detected independently.

10. The rapid analysis method according to claim 9, wherein for the plurality of sample separation loops arranged in parallel, step S2 is specifically:

s21, after all target gas components in the first sample injection separation loop enter the detector, switching the current separation column loop to a parallel second sample injection separation loop according to a set time interval, and ensuring that the gas components before the target gas components in the second sample injection separation loop are just discharged through reasonable process parameter setting, wherein the target gas components in the second sample injection separation loop enter the detector for analysis and detection after a shorter time interval;

s22, sequentially sending the target gas components separated in each sample injection separation loop into a detector for analysis and detection according to the method of the step S21, so as to realize continuous detection of the target gas components.