CN117269383A - Multi-type low Wen Duobu sweeping and concentrating device and sweeping and concentrating method thereof - Google Patents
Multi-type low Wen Duobu sweeping and concentrating device and sweeping and concentrating method thereof Download PDFInfo
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- CN117269383A CN117269383A CN202311142986.1A CN202311142986A CN117269383A CN 117269383 A CN117269383 A CN 117269383A CN 202311142986 A CN202311142986 A CN 202311142986A CN 117269383 A CN117269383 A CN 117269383A
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- 238000000034 method Methods 0.000 title claims description 11
- 238000010408 sweeping Methods 0.000 title description 5
- 239000007789 gas Substances 0.000 claims abstract description 101
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 80
- 239000007788 liquid Substances 0.000 claims abstract description 76
- 238000010926 purge Methods 0.000 claims abstract description 67
- 239000000126 substance Substances 0.000 claims abstract description 64
- 239000001307 helium Substances 0.000 claims abstract description 50
- 229910052734 helium Inorganic materials 0.000 claims abstract description 50
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims abstract description 50
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 41
- 239000012159 carrier gas Substances 0.000 claims abstract description 27
- 238000002347 injection Methods 0.000 claims abstract description 16
- 239000007924 injection Substances 0.000 claims abstract description 16
- 238000010201 enrichment analysis Methods 0.000 claims abstract description 10
- 238000001612 separation test Methods 0.000 claims abstract description 9
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 86
- 239000003345 natural gas Substances 0.000 claims description 43
- 238000004891 communication Methods 0.000 claims description 11
- 238000005070 sampling Methods 0.000 claims description 7
- 238000002844 melting Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 5
- 239000002912 waste gas Substances 0.000 claims description 4
- MPCRDALPQLDDFX-UHFFFAOYSA-L Magnesium perchlorate Chemical compound [Mg+2].[O-]Cl(=O)(=O)=O.[O-]Cl(=O)(=O)=O MPCRDALPQLDDFX-UHFFFAOYSA-L 0.000 claims description 3
- 239000003153 chemical reaction reagent Substances 0.000 claims description 3
- HUAUNKAZQWMVFY-UHFFFAOYSA-M sodium;oxocalcium;hydroxide Chemical compound [OH-].[Na+].[Ca]=O HUAUNKAZQWMVFY-UHFFFAOYSA-M 0.000 claims description 3
- 238000001514 detection method Methods 0.000 abstract description 3
- 108010063955 thrombin receptor peptide (42-47) Proteins 0.000 description 36
- 238000012360 testing method Methods 0.000 description 12
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- NMJORVOYSJLJGU-UHFFFAOYSA-N methane clathrate Chemical compound C.C.C.C.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O NMJORVOYSJLJGU-UHFFFAOYSA-N 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 5
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 3
- 229910002091 carbon monoxide Inorganic materials 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910001868 water Inorganic materials 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910001872 inorganic gas Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000012864 cross contamination Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005755 formation reaction Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/08—Preparation using an enricher
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention provides a multi-type low Wen Duobu purging and concentrating device, and particularly relates to the technical field of gas detection, wherein the multi-type low Wen Duobu purging and concentrating device comprises a sample injection unit and an enrichment analysis unit, wherein: the sample injection unit comprises a gas cylinder, a large-volume liquid cylinder, an automatic small-volume liquid cylinder, a chemical trap and a nitrogen source; the enrichment analysis unit comprises a first cold trap, a second cold trap, a third cold trap, a helium gas source and a GC carrier gas source; according to the invention, different low temperatures are set through the first cold trap, the second cold trap and the third cold trap to enrich components with different types and concentrations, after enrichment, the temperature rise and the purging are sequentially carried out on the first cold trap, the second cold trap and the third cold trap through helium gas, and the separation test is carried out by collecting the components off line, and the first cold trap, the second cold trap and the third cold trap can be continuously purged on line by using GC carrier gas, so that the efficiency is higher and more convenient when analyzing a large number of samples or samples with larger concentration differences.
Description
Technical Field
The invention relates to the technical field of gas detection, in particular to a multi-type low Wen Duobu purging and concentrating device and a purging and concentrating method thereof.
Background
Natural gas hydrate is a novel strategic resource in the 21 st century and is accepted as world-wide countryThe analysis of isotope geochemical data of gas molecules of the natural gas hydrate can reveal important information such as gas causes, sources, migration, mechanism of a storage process, formation and decomposition process control factors and the like, and has very important significance for exploring the reserves of the natural gas hydrate resources, the scale of a mineral deposit and the like, and the natural gas hydrate is formed in a low-temperature and high-pressure environment and comprises C1-C5 hydrocarbon gas molecules and CO 2 ，H 2 S，N 2 The method has the advantages that inorganic gas molecules such as Ar are complex, meanwhile, the content of the inorganic gas molecules is different, the influence of components and concentration is eliminated by multiple sample injection and sample injection quantity adjustment, so that the composition of isotopes is accurately obtained, and therefore, before gas-phase on-machine testing, the multi-component samples are purified, separated and collected through a pretreatment device and are accessed into an on-line testing system to analyze and detect the isotope values.
The existing carbon isotope testing technology of natural gas hydrate is mainly focused on the aspect of gas phase sample injection, for samples with larger component concentration difference, instruments and equipment can only be analyzed by a multi-column or fully enriched, separation and detection are carried out by a gas phase capillary column temperature programming method, for example, a conventional natural gas hydrate gas cylinder sample can reach the maximum concentration of 99.9%, the concentration of C2-C3 can reach the minimum concentration of 0.001%, when the carbon isotope test of similar samples is carried out, the multi-column or multi-time change of volume sample injection test is generally required, most of the operation schemes are in a manual sample injection mode at present, the test operation is time-consuming and the experimental efficiency is low, and multiple times of adjustment of the experimental scheme are also required to obtain the multi-component accurate carbon isotope value.
Disclosure of Invention
In order to solve the problems of time consumption in operation and low experimental efficiency caused by the need of adjusting an experimental scheme for analyzing a large number of samples or samples with large concentration differences of different types, the invention provides a multi-type low Wen Duobu purging and concentrating device and a purging and concentrating method thereof.
The invention is realized by the following technical scheme:
the invention provides a multi-type low Wen Duobu purging and concentrating device, which comprises a sample injection unit and an enrichment analysis unit, wherein:
the sample injection unit comprises a gas cylinder, a large-volume liquid cylinder, an automatic small-volume liquid cylinder, a chemical trap and a nitrogen source;
the enrichment analysis unit comprises a cold trap, wherein the cold trap comprises a first cold trap, a second cold trap, a third cold trap, a helium gas source and a GC carrier gas source;
natural gas in the gas cylinder or nitrogen enters a large-volume liquid cylinder and an automatic small-volume liquid cylinder to be purged, the natural gas enters the chemical trap, then enters the first cold trap, the second cold trap and the third cold trap to be cooled to different degrees, component samples with different types and different concentrations are respectively enriched in the first cold trap, the second cold trap and the third cold trap due to the difference of melting boiling points of components in the natural gas, after enrichment is completed, the first cold trap, the second cold trap and the third cold trap are rapidly heated, a helium source or a GC carrier gas source enters the first cold trap, the second cold trap and the third cold trap respectively to be purged, and the purged gas finally enters an offline manual collecting port to be collected or enters a gas phase sample inlet to be subjected to online separation test.
Further, a first electromagnetic valve and a first flow valve are sequentially communicated between the gas cylinder and the chemical trap, gas in the gas cylinder sequentially passes through the first electromagnetic valve and the first flow valve and enters the chemical trap, and the filling material of the chemical trap sequentially comprises magnesium perchlorate, a Roots reagent and soda lime.
Further, the automatic switching device further comprises a switching unit, wherein the switching unit comprises a first six-way valve, a second six-way valve, a third six-way valve and a first three-way valve, and the first six-way valve, the second six-way valve, the third six-way valve and the first three-way valve are sequentially communicated.
Further, two ends of the first cold trap are respectively communicated with a first six-way valve, two ends of the second cold trap are respectively communicated with a second six-way valve, two ends of the third cold trap are respectively communicated with a third six-way valve, the first six-way valve, the second six-way valve, the third six-way valve and the first three-way valve are sequentially communicated, gas treated by the chemical trap enters the first six-way valve and is discharged from the first six-way valve after passing through the first cold trap, and then enters the second six-way valve, and the helium gas in the helium gas source or the GC carrier gas source passes through the first six-way valve and the second six-way valve, the third six-way valve respectively enters the first cold trap, the second cold trap and the third cold trap are heated and purged, and finally the helium gas in the helium gas source or the GC carrier gas source enters the third three-way valve.
Further, the inlets of the helium source and the GC carrier gas source are respectively connected with a second electromagnetic valve, a third electromagnetic valve and a fourth electromagnetic valve, and helium enters the first cold trap, the second cold trap and the third cold trap through the second electromagnetic valve, the third electromagnetic valve and the fourth electromagnetic valve respectively.
Further, a second flow valve is further arranged on the helium inlet and is respectively communicated with the second electromagnetic valve, the third electromagnetic valve and the fourth electromagnetic valve, and helium enters the second electromagnetic valve, the third electromagnetic valve and the fourth electromagnetic valve through the second flow valve respectively.
Further, the device also comprises a fifth electromagnetic valve and a sixth electromagnetic valve, wherein the fifth electromagnetic valve is arranged between the large-volume liquid bottle and the chemical trap, the sixth electromagnetic valve is arranged between the automatic small-volume liquid bottle and the chemical trap, gas components in the large-volume liquid bottle enter the chemical trap through the fifth electromagnetic valve, and gas components in the automatic small-volume liquid bottle enter the chemical trap through the sixth electromagnetic valve.
Further, the automatic small-volume liquid bottle purging device further comprises a seventh electromagnetic valve, an eighth electromagnetic valve and a third flow valve, wherein one end of the seventh electromagnetic valve is communicated with the large-volume liquid bottle, the other end of the seventh electromagnetic valve is communicated with the third flow valve, one end of the eighth electromagnetic valve is communicated with the automatic small-volume liquid bottle, the other end of the eighth electromagnetic valve is communicated with the third flow valve, and nitrogen enters the automatic small-volume liquid bottle and the large-volume liquid bottle to be purged through the seventh electromagnetic valve and the eighth electromagnetic valve respectively.
Further, the device further comprises a cleaning unit, the cleaning unit comprises a ninth electromagnetic valve, a tenth electromagnetic valve and a pressure sensor, the pressure sensor is arranged between the chemical trap and the ninth electromagnetic valve, the tenth electromagnetic valve is arranged at the outlet of the third six-way valve, nitrogen enters the chemical trap through the ninth electromagnetic valve, and finally the nitrogen passes through the outlet of the third six-way valve and is emptied from the tenth electromagnetic valve at the outlet side of the third six-way valve.
Further, the purge concentration method of the multi-type low Wen Duobu purge concentration device comprises the following steps of:
natural gas or nitrogen of the gas cylinder enters the large-volume liquid bottle, natural gas components are purged from the automatic small-volume liquid bottle and enter the chemical trap, the natural gas components enter the chemical trap for treatment, then the natural gas components pass through the first cold trap, the second cold trap and the third cold trap in sequence, the first cold trap, the second cold trap and the third cold trap are rapidly cooled to different degrees according to the melting points of different types of gases, meanwhile, the components with low, medium and high concentration are enriched, the components which cannot be enriched and concentrated are discharged through the tenth electromagnetic valve, then the interfaces of the first six-way valve, the second six-way valve and the third six-way valve are switched, and the first cold trap, the second cold trap and the third cold trap are heated to room temperature, helium or GC carrier gas source enters the first cold trap, the second cold trap and the third cold trap respectively for purging, enriched components with different types and larger concentration difference are resolved according to sequence, and enter the first three-way valve through the outlet of the first six-way valve, the outlet of the second six-way valve and the outlet of the third six-way valve respectively for manual collection under selection lines to the air pocket collection or gas phase sample inlet for online next separation test, finally the first cold trap, the second cold trap and the third cold trap are rapidly heated, the ninth electromagnetic valve and the tenth electromagnetic valve are opened, and residual gas in the first cold trap, the second cold trap, the third cold trap and the pipeline is purged by nitrogen for exhausting waste gas.
The invention has the beneficial effects that:
(1) The multi-type low Wen Duobu purging concentration device provided by the invention is characterized in that the first cold trap, the second cold trap and the third cold trap are used for cooling and heating to complete enrichment purging, and when enrichment is carried out, the first cold trap, the second cold trap and the third cold trap are reduced to different temperatures; when purging, the first cold trap, the second cold trap and the third cold trap are quickly warmed to room temperature, natural gas in the liquid bottle or gas in the gas bottle is purged by nitrogen to cool and enrich through the first cold trap, the second cold trap and the third cold trap, helium is introduced into the first cold trap, the second cold trap and the third cold trap to be warmed and purged after enrichment is completed, and then the helium enters a three-way valve to be manually collected under a line to be selected to an air bag or a gas phase sample inlet for online separation test in the next step, and enrichment of components with larger concentration difference can be realized through temperature difference of the first cold trap, the second cold trap and the third cold trap, and a large number of samples or different types of samples can be processed simultaneously during the test.
(2) The multi-type low Wen Duobu purging and concentrating device provided by the invention has three sampling modes, namely, a large-volume liquid bottle, an automatic small-volume liquid bottle and a gas bottle are used for sampling, the large-volume liquid bottle is used for manual purging and sampling, the automatic small-volume liquid bottle is used for automatic purging and sampling, the gas bottle can be used for directly sampling natural gas, and the sampling mode has high flexibility.
(3) The multi-type low Wen Duobu purging concentration device provided by the invention is provided with the first three-way valve for switching, the GC carrier gas source and the helium source, when the first three-way valve is used for switching the manual collection port, the helium source is used for purging and blowing gas from the manual collection port to the gas supply bag for collection, when the first three-way valve is used for switching the gas phase sample inlet, the gas phase sample inlet is communicated with the instrument, the GC carrier gas source is used for purging the gas into the instrument and detecting the gas through the instrument, and the online collection test or the online carbon isotope test can be realized by switching the GC carrier gas source, the helium source and the first three-way valve.
(4) According to the multi-type low Wen Duobu purging concentration device, all three-way valves and electromagnetic valves can be controlled to be opened and closed through software, a cold trap can be controlled to be opened, closed, cooled and heated through software, sample injection and enrichment analysis can be automatically executed through software control, the operation efficiency of the whole device is improved, and manual switching is not needed in the whole process of automatic operation.
Drawings
FIG. 1 is a block diagram of a multi-type low Wen Duobu purge concentrator of the present invention;
in the figure: gas cylinder 1, bulk liquid bottle 2, automatic small-volume liquid bottle 3, chemical trap 4, first cold trap 5, second cold trap 6, third cold trap 7, first six-way valve 8, second six-way valve 9, third six-way valve 10, first flow valve 11, second flow valve 12, third flow valve 13, first solenoid valve 14, second solenoid valve 15, third solenoid valve 16, fourth solenoid valve 17, fifth solenoid valve 18, sixth solenoid valve 19, seventh solenoid valve 20, eighth solenoid valve 21, ninth solenoid valve 22, tenth solenoid valve 23, pressure sensor 24, first three-way valve 25;
the realization, functional characteristics and advantages of the present invention are further described with reference to the accompanying drawings in combination with the embodiments.
Detailed Description
In order to more clearly and completely describe the technical scheme of the invention, the invention is further described below with reference to the accompanying drawings.
Referring to fig. 1, the present invention provides a multi-type low Wen Duobu purge concentration device, which includes a sample injection unit and an enrichment analysis unit, wherein:
the sample injection unit comprises a gas cylinder 1, a large-volume liquid cylinder 2, an automatic small-volume liquid cylinder 3, a chemical trap 4 and a nitrogen source which are communicated in sequence;
the enrichment analysis unit comprises a cold trap, wherein the cold trap comprises a first cold trap 5, a second cold trap 6, a third cold trap 7, a helium gas source and a GC carrier gas source;
natural gas in the gas cylinder 1 or the nitrogen enters the large-volume liquid bottle 2 and the automatic small-volume liquid bottle 3 to be purged, the natural gas enters the chemical trap 4 and enters the first cold trap 5, the second cold trap 6 and the third cold trap 7 are cooled to different degrees, the first cold trap 5, the second cold trap 6 and the third cold trap 7 respectively enrich component samples with different types and different concentrations due to the difference of melting boiling points of components in the natural gas, after enrichment is completed, the first cold trap 5, the second cold trap 6 and the third cold trap 7 are rapidly heated, a helium source or a GC carrier gas source respectively enters the first cold trap 5, the second cold trap 6 and the third cold trap 7 to be purged, and the purged gas finally enters an off-line manual collection port to be collected or enters a gas phase sample inlet to be subjected to on-line separation test.
In the present embodiment, the following is described.
The nitrogen source is used for providing nitrogen for purging natural gas in the large-volume liquid bottle 2 and the automatic small-volume liquid bottle 3 and cleaning pipelines;
the helium source is used for providing helium for purging natural gas components enriched in the cold trap;
the GC carrier gas source is used for sweeping the natural gas component enriched in the cold trap and is used for separating chromatographic columns by instruments and equipment on line;
the gas cylinder 1 is used for storing and outputting natural gas components;
the large-volume liquid bottle 2 is used for manually purging and outputting natural gas components;
the first cold trap 5, the second cold trap 6 and the third cold trap 7 are used for cooling enrichment and heating purging;
the chemical trap 4 is used for removing water, carbon monoxide and carbon dioxide in the natural gas;
the automatic small-volume liquid bottle 3 is used for automatically purging and outputting natural gas components;
specifically, two sides of the chemical trap 4 are respectively provided with an inlet and an outlet, one end of the gas bottle 1 is sequentially connected with a first electromagnetic valve 14 and a first flow valve 11 and is communicated with the inlet of the chemical trap 4, a nitrogen source is connected with a third flow valve 13, the third flow valve 13 is provided with three pipelines, the first pipeline is sequentially connected with a seventh electromagnetic valve 20, a large-volume liquid bottle 2 and a fifth electromagnetic valve 18 from the inlet to the outlet side and is communicated with the inlet of the chemical trap 4, the second pipeline is sequentially connected with an eighth electromagnetic valve 21, an automatic small-volume liquid bottle 3 and a sixth electromagnetic valve 19 from the inlet to the outlet side and is communicated with a pipeline between the fifth electromagnetic valve 18 and the chemical trap 4, the third pipeline is sequentially connected with a ninth electromagnetic valve 22 and a pressure sensor 24 from the inlet to the outlet side and is communicated with a pipeline between the sixth electromagnetic valve 19 and the inlet of the chemical trap 4, the outlet end of the chemical trap 4 is connected with an interface 6 of the first six-way valve 8, the first six-way valve 8 interface 1 is sequentially connected with the first cold trap 5 and the first six-way valve 8 interface 4, the first six-way valve 8 interface 5 is connected with the second six-way valve 9 interface 6, the second six-way valve 9 interface 1 is sequentially connected with the second cold trap 6 and the second six-way valve 9 interface 4, the second six-way valve 9 interface 5 is connected with the third six-way valve 10 interface 6, the third six-way valve 10 interface 1 is sequentially connected with the third cold trap 7 and the third six-way valve 10 interface 4, the third six-way valve 10 interface 5 is connected with the tenth electromagnetic valve 23, the helium source is connected with the second flow valve 12, the inlet ends of the second electromagnetic valve 15, the third electromagnetic valve 16 and the fourth electromagnetic valve 17 are communicated with the flow valves, the outlet ends are respectively communicated with the first six-way valve 8 interface 2, the second six-way valve 9 interface 2 and the third six-way valve 10 interface 2, the first six-way valve 8 interface 3, the interface 3 of the second six-way valve 9 and the interface 3 of the third six-way valve 10 are jointly connected and collected on an outlet pipe, the outlet pipe is connected with the interface 1 of the first three-way valve 25, natural gas and nitrogen or nitrogen purged natural gas components enter the chemical trap 4, the first six-way valve 8, the second six-way valve 9 and the third six-way valve 10 are used for switching pipelines, different concentrations or different types of components are enriched on the first cold trap 5, the second cold trap 6 and the third cold trap 7, the first six-way valve 8, the second six-way valve 9 and the third six-way valve 10 are used for switching pipelines again, and helium is used for purging and collecting the first cold trap 5, the second cold trap 6 and the third cold trap 7, so that enrichment and purging are completed.
In one real-time mode: all three-way valves and solenoid valves can be controlled to be opened and closed through software, the cold trap can be controlled to be opened, closed, cooled and heated through software, sample injection and enrichment analysis can be automatically executed through software control, the operation efficiency of the whole device is improved, and manual switching is not needed.
Further, a first electromagnetic valve 14 and a first flow valve 11 are sequentially communicated between the gas cylinder 1 and the chemical trap 4, and gas in the gas cylinder 1 sequentially passes through the first electromagnetic valve 14 and the first flow valve 11 and enters the chemical trap 4, and the filling material of the chemical trap sequentially comprises magnesium perchlorate, a Roots reagent and soda lime.
In the present embodiment, the following is described.
The first solenoid valve 14 is used to open and close the gas cylinder 1;
the first flow valve 11 is used for controlling the flow of the gas cylinder 1;
specifically, the first electromagnetic valve 14 is opened to control the natural gas to enter the chemical trap 4, and the second flow valve 12 is used for adjusting the flow rate of the natural gas.
Further, the switching unit comprises a first six-way valve 8, a second six-way valve 9, a third six-way valve 10 and a first three-way valve, wherein the first six-way valve 8, the second six-way valve 9, the third six-way valve 10 and the first three-way valve are sequentially communicated, two ends of the first cold trap 5 are respectively communicated with the first six-way valve 8, two ends of the second cold trap 6 are respectively communicated with the second six-way valve 9, two ends of the third cold trap 7 are respectively communicated with the third six-way valve 10, the first six-way valve 8, the second six-way valve 9 and the third six-way valve 10 are sequentially communicated with the first three-way valve 25, gas processed by the chemical trap 4 enters the first six-way valve 8, is discharged from the first six-way valve 8 after passing through the first cold trap 5, then enters the second six-way valve 9, enters the second cold trap 6, is discharged from the second six-way valve 9, finally enters the third six-way valve 10, is discharged from the third cold trap 7, and finally enters the third cold trap 7, and finally passes through the third six-way valve 10, and finally enters the third cold trap 8, and finally passes through the third cold trap 7 and the third cold trap 8 and the third cold trap 6, and finally passes through the first six-way valve 25 and the six-way valve 7.
In the present embodiment, the following is described.
The first six-way valve 8, the second six-way valve 9 and the third six-way valve 10 are used for providing a switching structure for the separation and enrichment unit and the analysis and sample introduction unit;
the first three-way valve 25 is used for providing a switching structure for the purged gas to enter the off-line manual collection port or the on-line gas phase sample inlet;
specifically, the first three-way valve 25 is provided with three ports 1, 2 and 3, the port 2 of the first three-way valve 25 is a manual collection port, the port 3 of the first three-way valve 25 is a gas phase inlet, the manual collection port is used for connecting a gas bag, the gas phase inlet is used for connecting a testing instrument on line, the first six-way valve 8, the second six-way valve 9 and the third six-way valve 10 are respectively provided with six ports 1, 2,3, 4, 5 and 6, the ports 1, 3 and 5 are inlets, the ports 2, 4 and 6 are outlets, the first six-way valve 8, the second six-way valve 9 and the third six-way valve 10 are provided with two communication modes, one is 1,6, 5,4, 2,3 and the other is 2,1, 4,3, 6 and 5, and when the first communication mode is switched, gas in the chemical trap 4 sequentially enters the cold trap 1,6 of the first six-way valve 8, 4 and 5, the second six-way valve 9 and 6 are provided with two communication modes, the second cold trap 6, 4, 5 of the second six-way valve 9, 6, 1 of the third six-way valve 10, 4, 5 of the third cold trap 7, finally discharged from the tenth electromagnetic valve 23, the low concentration component, the medium concentration component and the high concentration component in the natural gas are respectively enriched on the first cold trap 5, the second cold trap 6 and the third cold trap 7, when the second medium communication mode is switched, helium gas respectively passes through the first cold trap 5, the second six-way valve 8 from 2,1 of the first six-way valve 8, the first cold trap 5,4, 3 of the first six-way valve 8 and the second six-way valve 9 from 2,1 of the second six-way valve 6, 4,3 of the second six-way valve 9 and the third six-way valve 10 from 2,1 of the third cold trap 7, 4,3 of the third six-way valve 10 are finally converged into the first three-way valve 25, the first three-way valve 25 is switched to enable gas to enter the gas pocket collection or the gas phase sample injection port for the next separation test, through switching the communication modes of the first six-way valve 8, the second six-way valve 9 and the third six-way valve 10, the functions of purging and enriching can be respectively realized through the first cold trap 5, the second cold trap 6 and the third cold trap 7, the sample treatment efficiency can be effectively improved, and the automatic purging and enriching can be realized.
Further, the inlets of the helium source and the GC carrier gas source are respectively connected with a second electromagnetic valve 15, a third electromagnetic valve 16 and a fourth electromagnetic valve 17, and helium enters the first cold trap 5, the second cold trap 6 and the third cold trap 7 through the second electromagnetic valve 15, the third electromagnetic valve 16 and the fourth electromagnetic valve 17.
In the present embodiment, the following is described.
The second electromagnetic valve 15 is used for opening and closing and controlling helium or GC carrier gas to purge the first cold trap 5;
the third solenoid valve 16 is used for opening and closing and controlling helium or GC carrier gas to purge the second cold trap 6;
the fourth electromagnetic valve 17 is used for opening and closing and controlling helium or GC carrier gas to purge the third cold trap 7;
specifically, the second solenoid valve 15, the third solenoid valve 16 and the fourth solenoid valve 17 can be opened and closed respectively to control the purging of helium or GC carrier gas, the purging of low-concentration components, medium-concentration components and high-concentration components can be performed respectively by opening the second solenoid valve 15, the third solenoid valve 16 and the fourth solenoid valve 17 respectively, and the purging can be performed simultaneously, the purging or the purging can be performed separately or together, one helium source and GC carrier gas source is selectively opened when the operation is performed, when the helium source is opened, helium gas is used for purging components with different concentrations, and the manual collection port of the interface 2 is switched by the first three-way valve 25 for collection, after collection, the offline test can be performed, when the GC carrier gas source is opened, the cold trap is purged by carrier gas, the interface 3 is switched by the first three-way valve 25 cold trap, the enriched sample enters the gas inlet and is analyzed by the direct chromatographic column of the instrument, and the better practicability is achieved.
Further, a second flow valve 12 is further arranged on the helium inlet, the second flow valve 12 is respectively communicated with a second electromagnetic valve 15, a third electromagnetic valve 16 and a fourth electromagnetic valve 17, and helium enters the second electromagnetic valve 15, the third electromagnetic valve 16 and the fourth electromagnetic valve 17 through the second flow valve 12.
In the present embodiment, the following is described.
The second flow valve 12 is used for controlling the flow of helium gas into the first cold trap 5, the second cold trap 6 and the third cold trap 7;
specifically, the second flow valve 12 is disposed at the helium inlet side, helium enters the first cold trap 5, the second cold trap 6 and the third cold trap 7 through the second solenoid valve 15, the third solenoid valve 16 and the fourth solenoid valve 17 through the flow valves, and the inflow amount of helium is controlled through the second flow valve 12 so as to control the purge concentration.
Further, the automatic small-volume liquid bottle further comprises a fifth electromagnetic valve 18 and a sixth electromagnetic valve 19, wherein the fifth electromagnetic valve 18 is arranged between the large-volume liquid bottle 2 and the chemical trap 4, the sixth electromagnetic valve 19 is arranged between the gas component in the automatic small-volume liquid bottle 3 and the chemical trap 4, the gas component in the large-volume liquid bottle 2 enters the chemical trap 4 through the fifth electromagnetic valve 18, and the automatic small-volume liquid bottle 3 enters the chemical trap 4 through the sixth electromagnetic valve 19.
In the present embodiment, the following is described.
The fifth electromagnetic valve 18 is used for controlling the opening and closing of a pipeline between the large-volume liquid bottle 2 and the chemical trap 4;
the sixth electromagnetic valve 19 is used for controlling the opening and closing of a pipeline between the automatic small-volume liquid bottle 3 and the chemical trap 4;
specifically, the fifth solenoid valve 18 and the sixth solenoid valve 19 are opened and closed and the natural gas component in the automatic small-volume liquid bottle 3 or the large-volume liquid bottle 2 is introduced into the chemical trap 4 by nitrogen purging.
Further, the automatic small-volume liquid bottle further comprises a seventh electromagnetic valve 20, an eighth electromagnetic valve 21 and a third flow valve 13, wherein one end of the seventh electromagnetic valve 21 is communicated with the large-volume liquid bottle 2, the other end of the seventh electromagnetic valve 21 is communicated with the third flow valve 13, one end of the eighth electromagnetic valve 21 is communicated with the automatic small-volume liquid bottle 3, the other end of the eighth electromagnetic valve 21 is communicated with the third flow valve 13, and nitrogen enters the automatic small-volume liquid bottle 3 and the large-volume liquid bottle 2 from the third flow valve 13 through the seventh electromagnetic valve 20 and the eighth electromagnetic valve 21 respectively.
In the present embodiment, the following is described.
The seventh electromagnetic valve 20 is used for controlling the pipeline between the nitrogen source and the large-volume liquid bottle 2 to be opened and closed;
the eighth electromagnetic valve 21 is used for controlling a pipeline between a nitrogen source and the automatic small-volume liquid bottle 3 to be opened and closed;
the third flow valve 13 is used for controlling the flow rate of the nitrogen source entering the space between the automatic small-volume liquid bottle 3 and the large-volume liquid bottle 2;
specifically, nitrogen enters the automatic small-volume liquid bottle 3 and the large-volume liquid bottle 2 through pipelines, a long needle pipeline is inserted into a natural gas component, nitrogen is introduced to purge gas in the bottle, natural gas is purged into the chemical trap 4 from the automatic small-volume liquid bottle 3 and the large-volume liquid bottle 2, the chemical trap 4 is used for removing carbon monoxide, carbon dioxide and water gas, and the seventh electromagnetic valve 20 and the eighth electromagnetic valve 21 can control and select to open pipelines between a nitrogen source and the automatic small-volume liquid bottle 3 and the large-volume liquid bottle 2 for sample purging.
Further, the device also comprises a cleaning unit, wherein the cleaning unit comprises a ninth electromagnetic valve 22, a tenth electromagnetic valve 23 and a pressure sensor 24, the pressure sensor 24 is arranged between the chemical trap 4 and the ninth electromagnetic valve 22, the tenth electromagnetic valve 23 is arranged at the outlet of the third six-way pipe, nitrogen enters the chemical trap 4 through the ninth electromagnetic valve 22, and finally flows out from the tenth electromagnetic valve 23 at the outlet side of the third six-way valve 10 through the outlet of the third six-way valve 10.
In the present embodiment, the following is described.
A ninth solenoid valve 22 is used to open and close the line from the nitrogen source to the inside of the chemical trap 4;
a tenth electromagnetic valve 23 for opening or closing a line between the outlets 5 of the sixth three-way valve;
the pressure sensor 24 is used for monitoring the pressure of a pipeline between the nitrogen source and the chemical trap 4 in real time;
specifically, the pressure valve can judge the tightness of the gas path, the ninth electromagnetic valve 22 and the tenth electromagnetic valve 23 are opened, the first cold trap 5, the second cold trap 6 and the third cold trap 7 are heated to 100 ℃, and the nitrogen sequentially passes through the ninth electromagnetic valve 22, the chemical trap 4, the first six-way valve 8, the first cold trap 5, the first six-way valve 8, the second six-way valve 9, the second cold trap 6, the second six-way valve 9, the third six-way valve 10 and the third cold trap 7 and is discharged to the outside from the tenth electromagnetic valve 23, and the nitrogen is filled into the chemical trap 4, the first cold trap 5, the second cold trap 6 and the third cold trap 7 to empty the internal gas, so that the waste gas is cleaned.
Further, a purge concentration method of a multi-type low Wen Duobu purge concentration device comprises the following steps: natural gas or nitrogen of the gas bottle 1 enters the large-volume liquid bottle 2, natural gas components are purged in the automatic small-volume liquid bottle 3 and enter the chemical trap 4, then the natural gas components pass through the first cold trap 5, the second cold trap 6 and the third cold trap 7 in sequence, the first cold trap 5, the second cold trap 6 and the third cold trap 7 are rapidly cooled to different degrees according to the melting boiling points of different types of gases, component samples with different types and different concentrations are respectively enriched, the components which cannot be enriched and concentrated are discharged through a tenth electromagnetic valve, then the first six-way valve 8, the second six-way valve 9 and the third six-way valve 10 are switched, the chemical trap 4 is closed to the loops 7 of the first cold trap 5, the second cold trap 6 and the third cold trap, meanwhile, the first cold trap 5, the second cold trap 6 and the third cold trap 7 are raised to room temperature, helium or GC carrier gas sources respectively enter the first cold trap 5, the second cold trap 6 and the third cold trap 7 for purging, different types of components are analyzed according to the carbon number sequence, respectively enter the first three-way valve 25 through the outlet of the first six-way valve 8, the outlet of the second six-way valve 9 and the outlet of the third six-way valve 10 for selecting a manual collecting port to collect the air bag or a gas phase sample inlet for further separation test, finally the first cold trap 5, the second cold trap 6 and the third cold trap 7 are rapidly raised in temperature, the ninth electromagnetic valve 22 and the tenth electromagnetic valve 23 are opened, and residual gases in pipelines are purged by nitrogen to empty waste gas.
Specifically, the seventh electromagnetic valve 20, the eighth electromagnetic valve 21 and the tenth electromagnetic valve 23 are closed, then the ninth electromagnetic valve 22 and the third flow valve 13 are opened to control the flow rate of nitrogen, the ninth electromagnetic valve 22 is closed after pressurizing for a period of time in a pipeline, the tightness of the gas path is detected through the change of the pressure sensor 24, and after the tightness of the gas path is detected, one of three modes is selected for sample injection: 1. the first solenoid valve 14 and the tenth solenoid valve 23 are opened, and the flow rate of the natural gas is controlled through the first flow valve 11; 2. the third flow valve 13, the fifth electromagnetic valve 18 and the seventh electromagnetic valve 20 are opened, and the large-volume liquid bottle 2 is purged by manual nitrogen; 3. the third flow valve 13, the sixth electromagnetic valve 19 and the eighth electromagnetic valve 21 are opened, the automatic nitrogen purging is selected to purge the automatic small-volume liquid bottle 3, natural gas components are introduced into the chemical trap 4, water, carbon monoxide and carbon dioxide gas in the natural gas are sequentially removed, then the natural gas is introduced into the first cold trap 5 of the first six-way valve 8, the second cold trap 6 of the second six-way valve 9 and the third cold trap 7 of the third six-way valve 10, the low temperature of the cold trap is related to the enriched components, the low temperature is sequentially reduced, when the enrichment is performed, the temperature of the first cold trap 5 is higher than the temperature of the second cold trap 6 and is higher than the temperature of the third cold trap 7, when the purging is performed, the natural gas is rapidly warmed to room temperature, the natural gas is sequentially introduced into the first cold trap 5, the second cold trap 6 and the third cold trap 7, and the temperature of the first cold trap 5, the second cold trap 6 and the third cold trap 7 are different, therefore, different concentration components can be enriched on the first cold trap 5, the second cold trap 6 and the third cold trap 7, components which cannot be enriched, such as oxygen, helium can be emptied through a tenth electromagnetic valve 23, after the enrichment of the different concentration components is completed, helium is selected to control the flow rate of helium or the source of GC carrier gas through a second flow valve 12, a six-way valve is switched, the first cold trap 5, the second cold trap 6 and the third cold trap 7 are warmed to room temperature, a fourth electromagnetic valve 17, a third electromagnetic valve 16 and a second electromagnetic valve 15 are sequentially opened, the first cold trap 5, the second cold trap 6 and the third cold trap 7 are purged, enriched samples are sequentially resolved, resolved gas is led to enter a manual collection port through a No. 1 port of a first three-way valve 25 for gas bag collection or a gas phase sample inlet for chromatographic column test, the invention switches the pipeline through the six-way valve and is matched with the cold trap to cool and raise the temperature to complete purging and enrichment, the invention can be applied to enrichment of different types and concentration gas samples, the rapid temperature raising and lowering of the cold trap can effectively separate samples through the difference of the boiling points of components, and reduce the risk of cross contamination of the samples, the full-automatic separation can be realized through the six-way valve, the electromagnetic valve and the flow valve, the manual operation can be completely replaced, and the working parameters can be selected according to the actual conditions.
Of course, the present invention can be implemented in various other embodiments, and based on this embodiment, those skilled in the art can obtain other embodiments without any inventive effort, which fall within the scope of the present invention.
Claims (10)
1. The utility model provides a many types are low Wen Duobu sweeps enrichment facility which characterized in that, includes sampling unit and enrichment analysis unit, wherein:
the sample injection unit comprises a gas cylinder, a large-volume liquid cylinder, an automatic small-volume liquid cylinder, a chemical trap and a nitrogen source;
the enrichment analysis unit comprises a cold trap, wherein the cold trap comprises a first cold trap, a second cold trap, a third cold trap, a helium gas source and a GC carrier gas source;
natural gas in the gas cylinder or nitrogen enters a large-volume liquid bottle and an automatic small-volume liquid bottle to be purged, natural gas enters the chemical trap, then enters the first cold trap, the second cold trap and the third cold trap to be cooled to different degrees, the first cold trap and the second cold trap enrich component samples with different types and different concentrations respectively due to the difference of melting boiling points of components in the natural gas, after enrichment is completed, the first cold trap, the second cold trap and the third cold trap are rapidly warmed, a helium source or a GC carrier gas source enters the first cold trap, the second cold trap and the third cold trap respectively to be purged, and the purged gas finally enters an offline manual collection port to be collected or enters a gas phase sample inlet to be subjected to a next separation test on line.
2. The multi-type low-temperature automatic multi-step purging concentration device according to claim 1, wherein a first electromagnetic valve and a first flow valve are sequentially communicated between the gas cylinder and the chemical trap, gas in the gas cylinder sequentially passes through the first electromagnetic valve and the first flow valve and enters the chemical trap, and the filling sequence of the chemical trap is magnesium perchlorate, a Roots reagent and soda lime.
3. The multi-type low Wen Duobu purge concentration device of claim 2, further comprising a switching unit comprising a first six-way valve, a second six-way valve, a third six-way valve, and a first three-way valve, wherein the first six-way valve, the second six-way valve, the third six-way valve, and the first three-way valve are in sequential communication.
4. A multi-type low Wen Duobu purge concentration device according to claim 3, wherein two ends of the first cold trap are respectively communicated with a first six-way valve, two ends of the second cold trap are respectively communicated with a second six-way valve, two ends of the third cold trap are respectively communicated with a third six-way valve, the first six-way valve, the second six-way valve and the third six-way valve are sequentially communicated with the first three-way valve, gas processed by a chemical trap enters the first six-way valve and is discharged from the first six-way valve after passing through the first cold trap, then enters the second six-way valve and enters the second cold trap, is discharged from the second six-way valve, finally enters the third six-way valve, is enriched through the third cold trap, and finally gas which cannot be enriched by different temperatures of the third cold trap is discharged to the outside from the third six-way valve, and the gas source or the GC carrier is discharged from the first six-way valve, the second six-way valve, the third cold trap and the third cold trap, and finally enters the third cold trap, and the purge device respectively.
5. The multi-type low Wen Duobu purge concentrator of claim 4, wherein said helium source and said GC carrier source have respective inlets to which are connected a second solenoid valve, a third solenoid valve, and a fourth solenoid valve through which helium enters said first cold trap, said second cold trap, and said third cold trap, respectively.
6. The multi-type low Wen Duobu purge concentrator of claim 5, further comprising a second flow valve in communication with said second, third and fourth solenoid valves, respectively, wherein said helium gas is admitted into said second, third and fourth solenoid valves through said second flow valve, respectively.
7. The multi-type low Wen Duobu purge concentrator of claim 1, further comprising a fifth solenoid valve disposed between said bulk liquid bottle and said chemical trap and a sixth solenoid valve disposed between said automatic small volume liquid bottle and said chemical trap, wherein gaseous components within said bulk liquid bottle enter said chemical trap through said fifth solenoid valve and gaseous components within said automatic small volume liquid bottle enter said chemical trap through said sixth solenoid valve.
8. The multi-type low Wen Duobu purge concentration device of claim 1, further comprising a seventh solenoid valve having one end in communication with the bulk liquid bottle and the other end in communication with the third flow valve, an eighth solenoid valve having one end in communication with the automatic small volume liquid bottle and the other end in communication with the third flow valve, and a third flow valve from which nitrogen enters into the automatic small volume liquid bottle and the bulk liquid bottle purge through the seventh solenoid valve, the eighth solenoid valve, respectively.
9. The multi-type low Wen Duobu purge concentrator of claim 8, further comprising a purge unit comprising a ninth solenoid valve, a tenth solenoid valve, and a pressure sensor, said pressure sensor being disposed between said chemical trap and said ninth solenoid valve, said tenth solenoid valve being disposed at an outlet of said third six-way valve, nitrogen entering said chemical trap through said ninth solenoid valve, and finally exiting through an outlet of said third six-way valve and from said tenth solenoid valve on an outlet side of said third six-way valve.
10. A method of purge concentration of a multi-type low Wen Duobu purge concentration device according to any one of claims 1 to 9, comprising the steps of:
natural gas or nitrogen of the gas cylinder enters the large-volume liquid bottle, natural gas components are purged from the automatic small-volume liquid bottle and enter the chemical trap, the natural gas components enter the chemical trap for treatment, then the natural gas components pass through the first cold trap, the second cold trap and the third cold trap in sequence, the first cold trap, the second cold trap and the third cold trap are rapidly cooled to different degrees according to the melting points of different types of gases, meanwhile, the components with low, medium and high concentration are enriched, the components which cannot be enriched and concentrated are discharged through the tenth electromagnetic valve, then the interfaces of the first six-way valve, the second six-way valve and the third six-way valve are switched, and the first cold trap, the second cold trap and the third cold trap are heated to room temperature, helium or GC carrier gas source enters the first cold trap, the second cold trap and the third cold trap respectively for purging, enriched components with different types and larger concentration difference are resolved according to sequence, and enter the first three-way valve through the outlet of the first six-way valve, the outlet of the second six-way valve and the outlet of the third six-way valve respectively for manual collection under selection lines to the air pocket collection or gas phase sample inlet for online next separation test, finally the first cold trap, the second cold trap and the third cold trap are rapidly heated, the ninth electromagnetic valve and the tenth electromagnetic valve are opened, and residual gas in the first cold trap, the second cold trap, the third cold trap and the pipeline is purged by nitrogen for exhausting waste gas.
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