CN218212809U - Gas chromatography analysis system for coal chemical industry conversion gas - Google Patents
Gas chromatography analysis system for coal chemical industry conversion gas Download PDFInfo
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- CN218212809U CN218212809U CN202222581339.8U CN202222581339U CN218212809U CN 218212809 U CN218212809 U CN 218212809U CN 202222581339 U CN202222581339 U CN 202222581339U CN 218212809 U CN218212809 U CN 218212809U
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Abstract
Gas chromatography analytic system that coal industry becomes gas, the utility model belongs to the technical field of the detection technology and specifically relates to a gas chromatography analytical technique equipment that coal industry becomes gas. The gas chromatography analysis system of the coal chemical industry conversion gas comprises a ten-way valve V1, a six-way valve V2, a chromatographic column 1, a chromatographic column 2, a chromatographic column 3, a TCD detector, a quantitative tube, a resistance valve 1 and a resistance valve 2. The utility model discloses a system adopts ten logical valve blowbacks to advance kind technique, realizes heavy ends blowback function. When the required components enter the separation column, the unnecessary components in the pre-column are blown back out of the chromatographic column to be discharged, so that the heavy components are prevented from entering the post-system to pollute the chromatographic column and the detector. The six-way valve is connected in series and the bypass is selected, so that one-time sample injection is realized, the required components are separated at one time, and the content of the components is obtained. The analysis process avoids pollution and the result is accurate.
Description
Technical Field
The utility model belongs to the technical field of the detection technique and specifically relates to a gas chromatography analysis technical equipment that coal industry becomes gas changes.
Background
The coal chemical industry transformation gas contains argon, nitrogen, methane, carbon monoxide, carbon dioxide, hydrogen sulfide, carbonyl sulfide, hydrogen, organic sulfur and other small amounts of unknown heavy component compounds. In general, the shift gas is primarily concerned with argon, nitrogen, methane, carbon monoxide, carbon dioxide, hydrogen sulfide and carbonyl sulfide. The hydrogen content can be calculated by subtraction. The total amount of other heavy component compounds such as organic sulfur, ethanol, ammonia and the like does not exceed 0.5%, so that the influence on the content of the measured other components is not large, and the control on the production process is not substantial, but although the control on the production process is not substantial, the heavy component compounds can cause the pollution of systems such as chromatographic columns, detectors and the like after entering a gas chromatograph, thereby damaging analytical instruments.
In addition, the argon, nitrogen and carbon monoxide in the converted gas need to be separated by using a 5A molecular sieve chromatographic column, however, if carbon dioxide, hydrogen sulfide and the like in the converted gas enter the 5A molecular sieve, irreversible adsorption occurs, and the chromatographic column is damaged. Therefore, conventional monochromatic column separation techniques have not been able to perform analytical detection of transformed gas components.
Therefore, the connection structure of the detection system needs to be changed based on the influence and damage of the heavy component compounds, carbon dioxide, and hydrogen sulfide gas in the converted gas on the detection system.
SUMMERY OF THE UTILITY MODEL
The utility model provides a gas chromatography analytic system of coal industry change gas through setting up two valves three posts, realizes once advancing the appearance, and the disposable separation of required component records its content.
The gas chromatography analysis system of the coal chemical industry transformation gas comprises a ten-way valve V1, a six-way valve V2, a chromatographic column 1, a chromatographic column 2, a chromatographic column 3, a TCD detector, a quantitative tube, a resistance valve 1 and a resistance valve 2;
the ten-way valve V1 is provided with 10 interfaces which are 1-10 respectively; the six-way valve V2 is provided with 6 interfaces which are respectively 1-6;
the resistance valve 1 and the resistance valve 2 are two needle valves which are respectively arranged on the ten-way valve V1 and the six-way valve V2, the resistance valve 1 is connected with a connector 6 of the ten-way valve V1, and the resistance valve 2 is connected between connectors 5 and 4 of the six-way valve V2;
the carrier gas 1 and the carrier gas 2 are respectively connected to the interface 2 of the ten-way valve V1 and the interface 5;
the quantitative pipe is communicated with the interface 8 and the interface 1 of the ten-way valve V1;
the sample enters from a port 9 of the ten-way valve V1 and exits from a port 10 of the ten-way valve V1;
the TCD detector is connected to the interface 3 of the six-way valve V2.
The ten-way valve V1 is used for gas sample injection and back flushing, and the six-way valve V2 is used for enabling sample gas to selectively pass through the chromatographic column 3 or enter the detector through a bypass.
The ten-way valve V1, the six-way valve V2, the chromatographic column, the quantitative tube and the sample replacement pipeline are all subjected to silanization treatment, so that the adsorption of hydrogen sulfide gas is avoided.
The chromatographic column 1 is a silanization treated Porapak N stainless steel packed column with the diameter of 3-4mm 0.5-1.5m, and the chromatographic column 2 is a silanization treated Porapak N stainless steel packed column with the diameter of 3-4mm 1.5-2.5 m; the chromatographic column 3 is a 5A molecular sieve stainless steel packed column with phi 3-4mm x 4-7 m.
The carrier gas 1 is high-purity hydrogen gas 25-40mL/min, and the carrier gas 2 is high-purity hydrogen gas 25-40mL/min.
The utility model discloses a system adopts ten logical valve blowbacks to advance kind technique, realizes heavy ends blowback function. When the needed components enter the separation column, the components which are not needed in the pre-column are reversely blown out of the chromatographic column to be discharged, so that the heavy components are prevented from entering a rear system to pollute the chromatographic column and the detector. Realize one-time sample introduction, separate the needed components at one time and obtain the content of the components. The analysis process avoids pollution and the result is accurate.
And (3) switching by adopting a six-way valve to realize the separation of argon, nitrogen, methane and carbon monoxide on a 5A column, and separating the rest components harmful to the 5A molecular sieve: the carbon dioxide, the hydrogen sulfide and the carbonyl sulfide enter the detector from the bypass after being separated by the P-N chromatographic column, so that the carbon dioxide, the hydrogen sulfide and the like are prevented from entering the 5A chromatographic column to cause the damage of the chromatographic column.
And the silanization-treated chromatographic column, the sample introduction valve and the sample replacement pipeline are used, so that the hydrogen sulfide gas is prevented from being adsorbed, and the accuracy of an analysis result is ensured.
The separation temperature of 100-120 ℃ is adopted, so that the system is prevented from being polluted by condensation of water in the sample.
Drawings
Fig. 1 is the structure schematic diagram of the initial replacement + series connection and the back-blowing + series connection state of the present invention.
Fig. 2 is the structure diagram of the sample injection + series connection state of the present invention.
Fig. 3 is the structure diagram of the sample injection + bypass state of the present invention.
Fig. 4 is the schematic structural diagram of the back-flushing + bypass state of the present invention.
Detailed Description
Example 1: the gas chromatography analysis system of the coal chemical industry transformation gas comprises a ten-way valve V1, a six-way valve V2, a chromatographic column 1, a chromatographic column 2, a chromatographic column 3, a TCD detector, a quantitative tube, a resistance valve 1 and a resistance valve 2;
the ten-way valve V1 is provided with 10 interfaces which are 1-10 respectively; the six-way valve V2 is provided with 6 interfaces which are respectively 1-6 interfaces;
the resistance valve 1 and the resistance valve 2 are two needle valves which are respectively arranged on the ten-way valve V1 and the six-way valve V2, the resistance valve 1 is connected with a connector 6 of the ten-way valve V1, and the resistance valve 2 is connected between connectors 5 and 4 of the six-way valve V2;
the carrier gas 1 and the carrier gas 2 are respectively connected to the interface 2 and the interface 5 of the ten-way valve V1;
the quantitative pipe is communicated with the interface 8 and the interface 1 of the ten-way valve V1;
the sample enters from a port 9 of the ten-way valve V1 and exits from a port 10 of the ten-way valve V1;
the TCD detector is connected to interface 3 of the six-way valve V2.
The ten-way valve V1 is used for gas sample injection and back flushing, and the six-way valve V2 is used for enabling sample gas to selectively pass through the chromatographic column 3 or enter the detector through a bypass.
The ten-way valve V1, the six-way valve V2, the chromatographic column, the quantitative tube and the sample replacement pipeline are all subjected to silanization treatment, so that the adsorption of hydrogen sulfide gas is avoided.
The chromatographic column 1 is a silanized Porapak N stainless steel packed column with the diameter of 3mm x 1.2m, and the chromatographic column 2 is a silanized Porapak N stainless steel packed column with the diameter of 3mm x 2m; the column 3 was a 5A molecular sieve stainless steel packed column with diameter 3mm x 6 m. The separation temperature of the chromatographic column is 100 ℃, and the chromatographic column is prevented from being polluted by moisture condensation.
The carrier gas 1 is high-purity hydrogen gas 30mL/min, and the carrier gas 2 is high-purity hydrogen gas 30mL/min.
The resistance valve 1 provides the pressure sum of the chromatographic column 2 and the chromatographic column 3, so that the pressure reduction of a gas path system caused by resistance reduction after valve cutting and back flushing is avoided, and the chromatograph cannot normally operate. The resistance valve 2 provides the same pressure as the column 3, ensuring that the carrier gas flow rate is stable after switching to bypass.
The whole process of system usage, i.e. analysis of one sample, goes through five states, respectively:
1. initial permutation + series state
In this state, the system pipe connection structure is as shown in fig. 1. In this state, the ports 10-1, 2-3, 4-5, 6-7, 8-9 of the ten-way valve V1 are in the communicating state, and the ports 6-1, 2-3, 4-5 of the six-way valve V2 are in the communicating state. The sample gas enters through a port 9 in a ten-way valve V1, flows out of a port 10 after replacing a quantitative tube, the carrier gas 1 enters through a port 2 in the ten-way valve V1, is discharged through a resistance valve 1 after reversely blowing the chromatographic column 1, the carrier gas 2 enters through a port 5 in the ten-way valve V1, and enters into a TCD detector after passing through a chromatographic column 2 and a chromatographic column 3 through a port 4, so that a corresponding chromatogram is obtained.
The TCD detector in the initial state obtains a baseline value of pure carrier gas passing through the chromatographic columns 2 and 3, which is the initial detection value before the sample detection.
2. Sample introduction + series connection state
In this state, the system pipe connection structure is as shown in fig. 2. In this state, the ports 1-2, 3-4, 5-6, 7-8, 9-10 of the ten-way valve V1 are in the communicating state, and the ports 6-1, 2-3, 4-5 of the six-way valve V2 are in the communicating state. Sample gas enters through a ten-way valve V1 port 9 and exits at 10. The carrier gas 1 enters through a connector 2 of a ten-way valve V1, the sample gas in the quantitative tube is brought into the chromatographic column 1 for pre-separation, then is continuously brought into the chromatographic column 2 for further separation, and hydrogen, argon, nitrogen, carbon monoxide and methane are sent into the chromatographic column 3, the carrier gas 2 enters through a connector 5 of the ten-way valve V1 and is discharged through a connector 6 and a resistance valve 1.
In the further separation process of the chromatographic column 2, hydrogen, argon, nitrogen, carbon monoxide and methane are firstly separated from the chromatographic column 2 and enter the chromatographic column 3, and after the hydrogen, argon, nitrogen, carbon monoxide and methane enter the chromatographic column 3, the sample injection and bypass state is started to prevent the three components of carbon dioxide, hydrogen sulfide and carbonyl sulfide from entering the chromatographic column 3. The time for opening the sample injection and the bypass needs to be pretested before the formal sample detection, and the time for hydrogen, argon, nitrogen, carbon monoxide and methane in the sample to enter the chromatographic column 3 is determined. And determining the time of opening the sample injection and bypass state by using the time.
3. Sample introduction + bypass state
In this state, the system pipe connection structure is as shown in fig. 3. In this state, the ports 1-2, 3-4, 5-6, 7-8, 9-10 of the ten-way valve V1 are in the connected state, and the ports 1-2, 3-4, 5-6 of the six-way valve V2 are in the connected state. The sample gas enters through port 9 of the ten-way valve V1 and exits at 10. Carrier gas 1 enters through a connector 2 of a ten-way valve V1, sample gas in a quantitative tube is brought into a chromatographic column 1 for pre-separation, then is continuously brought into the chromatographic column 2 for further separation, after hydrogen, argon, nitrogen, carbon monoxide and methane are sent into the chromatographic column 3, when other substances such as carbon dioxide and the like are about to flow out from the chromatographic column 2, the six-way valve V2 is switched into a bypass, the hydrogen, the argon, the nitrogen, the carbon monoxide and the methane enter a detector through connectors 6, 5, 4 and 3 of the six-way valve V2, the carbon dioxide, hydrogen sulfide and carbonyl sulfide enter the detector through the bypass to obtain a corresponding chromatogram, the carrier gas 2 enters through the connector 5 of the ten-way valve V1 and is emptied through a resistance valve 1 through 6.
4. Back-flushing + bypass state
In this state, the system pipe connection structure is as shown in fig. 4. In this state, the ports 10-1, 2-3, 4-5, 6-7, 8-9 of the ten-way valve V1 are in the communicating state, and the ports 1-2, 3-4, 5-6 of the six-way valve V2 are in the communicating state. The carrier gas 1 enters through the interface 2 of the ten-way valve V1, the chromatographic column 1 is blown back and then is discharged through the resistance valve 1, the carrier gas 2 enters through the interface 5 of the ten-way valve V1, and components in the chromatographic column 2 are brought into the detector to obtain a corresponding chromatogram.
In this state, after methane, carbon dioxide, and carbonyl sulfide flow out of the column 1 and enter the column 2, the time for carbonyl sulfide to flow out of the column 1 is calculated from the carbonyl sulfide peak time and the column length measured in the preliminary test before the detection of the main sample, and the back flushing time is set. And the carrier gas 1 of the ten-way valve V1 is subjected to back blowing, so that impurity groups behind carbonyl sulfide in the chromatographic column 1 can be blown out of the system in a back blowing manner, and the phenomenon that the chromatographic column and a detector are polluted by the entering system is avoided.
5. Back-flushing + series state
In this state, the system pipe connection structure is as shown in fig. 1. In this state, the ports 10-1, 2-3, 4-5, 6-7, 8-9 of the ten-way valve V1 are in the communicating state, and the ports 6-1, 2-3, 4-5 of the six-way valve V2 are in the communicating state. The sample gas enters through a port 9 in a ten-way valve V1, flows out from a port 10 after replacing a quantitative tube, the carrier gas 1 enters through a port 2 in the ten-way valve V1, is discharged through a resistance valve 1 after back flushing the chromatographic column 1, the carrier gas 2 enters through ports 5 and 4 in the ten-way valve V1, and is separated from the hydrogen, argon, nitrogen, carbon monoxide and methane remained in the chromatographic column 3 and then brought into a TCD detector after passing through the chromatographic column 2 and the chromatographic column 3, so that a corresponding chromatogram is obtained.
Claims (4)
1. The gas chromatography analysis system of the coal chemical industry conversion gas comprises a ten-way valve V1, a six-way valve V2, a chromatographic column 1, a chromatographic column 2, a chromatographic column 3, a TCD detector, a quantitative tube, a resistance valve 1 and a resistance valve 2;
the ten-way valve V1 is provided with 10 interfaces which are 1-10 respectively; the six-way valve V2 is provided with 6 interfaces which are respectively 1-6 interfaces;
the resistance valve 1 and the resistance valve 2 are two needle valves which are respectively arranged on the ten-way valve V1 and the six-way valve V2, the resistance valve 1 is connected with a connector 6 of the ten-way valve V1, and the resistance valve 2 is connected between connectors 5 and 4 of the six-way valve V2;
the carrier gas 1 and the carrier gas 2 are respectively connected to the interface 2 of the ten-way valve V1 and the interface 5;
the quantitative pipe is communicated with the interface 8 and the interface 1 of the ten-way valve V1;
the sample enters from a port 9 of the ten-way valve V1 and exits from a port 10 of the ten-way valve V1;
the TCD detector is connected to the interface 3 of the six-way valve V2.
2. The gas chromatographic analysis system of the coal chemical industry shift gas as recited in claim 1, characterized in that the ten-way valve V1 is used for gas sample injection and back flushing, and the six-way valve V2 is used for sample gas to selectively pass through the chromatographic column 3 or enter the detector through a bypass.
3. The gas chromatography analysis system for coal chemical industry shift gas according to claim 1, characterized in that the ten-way valve V1, the six-way valve V2, the chromatographic column, the quantitative tube, and the sample replacement pipeline are all subjected to silanization.
4. The gas chromatographic analysis system for coal chemical industry converted gas according to claim 1, characterized in that the chromatographic column 1 is a silanized Porapak N stainless steel packed column with a diameter of 3-4mm 0.5-1.5m, and the chromatographic column 2 is a silanized Porapak N stainless steel packed column with a diameter of 3-4mm 1.5-2.5 m; the chromatographic column 3 is a 5A molecular sieve stainless steel packed column with the diameter of 3-4mm 4-7 m.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202222581339.8U CN218212809U (en) | 2022-09-28 | 2022-09-28 | Gas chromatography analysis system for coal chemical industry conversion gas |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202222581339.8U CN218212809U (en) | 2022-09-28 | 2022-09-28 | Gas chromatography analysis system for coal chemical industry conversion gas |
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| Publication Number | Publication Date |
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| CN218212809U true CN218212809U (en) | 2023-01-03 |
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| CN202222581339.8U Active CN218212809U (en) | 2022-09-28 | 2022-09-28 | Gas chromatography analysis system for coal chemical industry conversion gas |
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