CN102323359B - Preparative gas chromatography system and method for separating inert gas sample thereof - Google Patents
Preparative gas chromatography system and method for separating inert gas sample thereof Download PDFInfo
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Abstract
The invention relates to a preparative gas chromatography system and a method for separating an inert gas sample thereof. The sampling and sample injection are controlled by a large-volume sample quantitative ring combined with a pneumatic six-way valve; a method of high temperature desorption of components in an enriching column combined with diaphragm supercharging diffusion transfer is adopted; enriching columns with different fillers are adopted for different gas; and independent enrichment of multi-target components is realized. The invention solves the technical problems that large-volume and large-scale sample injection, collection and preparation are difficult to realize in current gas chromatography systems and applications thereof, and increases the production efficiency.
Description
Technical field
The present invention relates to a kind of gas chromatography piece-rate system and gas chromatography piece-rate system for separating of the method for inert gas sample, particularly a kind of preparative gas chromatography system and prepare the method for inert gas sample.
Background technology
Gas chromatography is a kind of analysis means of routine, is roughly divided into analytic type gas chromatography and the large class of preparative gas chromatography two application purpose, and wherein the development of analytic type gas chromatography and application have reached a kind of degree of maturation.Preparative scale chromatography is identical with the ultimate principle of analytic type chromatogram, but also there is significant difference, analytic type chromatogram requires less sample introduction or trace sample introduction, be conducive to form symmetrical chromatographic peak, reduce hangover, preparative scale chromatography is under the prerequisite of the product purity that guarantees to reach certain and yield, requires to improve sample size and the product volume of chromatographic column.The principal element of restriction preparative gas chromatography technical development is to be difficult to realize the large-scale sample feeding of large volume, collection and preparation at present, causes production efficiency lower.
Summary of the invention
The object of the invention is to provide a kind of method of preparative gas chromatography system and separated inert gas sample thereof, it has solved the technical matters that is difficult to realize the large-scale sample feeding of large volume, collection and preparation existing in existing gas chromatography system and application thereof, has improved production efficiency.
Technical solution of the present invention is:
A kind of preparative gas chromatography system, comprise gas boosting sampling device, preparative gas chromatography separation control device, gas composition collection and preparation facilities and vacuum pump, its special character is: described gas boosting sampling device comprises that sample quantitatively encircles, the first membrane pump, pneumatic six-way valve; The import of described the first membrane pump communicates with sample source bottle by valve, and its outlet communicates with the b end of pneumatic six-way valve by valve; The described sample quantitatively two ends of ring communicates with f end and the c end of pneumatic six-way valve respectively; Described pneumatic six-way valve comprises pneumatic six-way valve valve body and drives gas, and described driving gas provides power for the switching of the pneumatic six-way valve of pneumatic six-way valve between sampling and sample introduction state; Described preparative gas chromatography separation control device comprises chromatogram main control system, chromatographic column, chromatographic detector, carrier gas bottle; Described carrier gas bottle communicates with the e end of pneumatic six-way valve by valve; The import of described chromatographic column communicates with the d of pneumatic six-way valve end, and its outlet communicates with the entrance of chromatographic detector; Described gas composition is collected with preparation facilities and is comprised enrichment unit, the second membrane pump, component receiving flask and the cold-trap with temperature regulating device; The entrance of described enrichment unit communicates with the outlet of chromatographic detector by valve, the outlet of described enrichment unit communicates with the entrance of the second membrane pump by valve, described the second barrier film delivery side of pump communicates with the entrance of component receiving flask in cold-trap, and the outlet of described component receiving flask communicates with the entrance of enrichment unit by valve; The bleeding point of described vacuum pump by threeway after, the valve of leading up to communicates with sample source bottle and the first membrane pump entrance of gas boosting sampling device, and the valve of separately leading up to communicates with outlet and the second membrane pump entrance of the enrichment unit 10 of preparation facilities with gas composition collection.
Between above-mentioned sample source bottle 3 and the first membrane pump 1, between the b end of the first membrane pump and pneumatic six-way valve 7, between chromatographic detector and enrichment unit, be respectively arranged with the pressure gauge of monitoring pipeline gaseous tension.
Above-mentioned enrichment unit is the enriching column of single enriching column or a plurality of parallel connections.
Above-mentioned chromatographic column is 5
molecular sieve packed column, column internal diameter is 4mm, column length is 12m; Above-mentioned detecting device is large volume thermal conductivity cell detector; Above-mentioned carrier gas is high pure nitrogen; Above-mentioned enriching column filler is graininess cocoanut active charcoal, and granularity of activated carbon is 14～20 orders.
Method with the separated inert gas sample of above-mentioned preparative gas chromatography system, comprises the following steps:
1] sample feeding:
1.1] access sample source bottle, keeps it to carry valve closing;
1.2] switch pneumatic six-way valve, make sample quantitatively encircle and be operated under sampling state, the quantitative ring of sample and auxiliary piping thereof are evacuated to below 10Pa;
1.3] open the valve that carries of sample source bottle, utilize membrane pump that sample gas is transferred to the quantitative ring of sample from sample source bottle;
1.4] switch pneumatic six-way valve, sample is quantitatively encircled in sample introduction state;
1.5] utilize carrier gas will quantitatively encircle in sample be written into chromatographic column, the pressure during simultaneously with pressure gauge indication sample introduction;
2] component separation and enrichment:
2.1] adopt the calibrating gas of target components, determine optimization chromatographic condition and the sensors work parameter of component separation, set up chromatographic applications program;
2.2], in the chromatographic applications program of setting up, determine the chromatographic retention of each target components;
2.3] start chromatographic applications program, according to the retention time of fixed each component, control the three-way switch valve of detecting device rear end, target components is switched to corresponding enriching column and carries out enrichment;
3] component desorb:
After component enrichment finishes, enriching column is heated to be not less than 200 ℃ under closed state, and constant temperature 10min, make target components desorb completely from enriching column;
4] component shifts:
Adopt membrane pump, desorb component in enriching column is transferred in component receiving flask, open the circulation gas circuit between receiving flask and enriching column, rinse enriching column;
5] component rectifying and sample preparation:
5.1] by cold-trap, the temperature of component receiving flask is down to below the boiling point of target components, makes target components completely in condensing state;
5.2] unlatching vacuum pump is emptying by the residual gas component in sample source bottle, the concentrated collection of realize target component.
Above-mentioned chromatographic column is 5
molecular sieve packed column, column internal diameter is 4mm, column length is 12m; Above-mentioned detecting device is large volume thermal conductivity cell detector; Above-mentioned carrier gas is high pure nitrogen; Above-mentioned enriching column is active carbon filler enriching column.
The beneficial effect that the present invention has:
1, the present invention adopts the quantitative loops of sample of large volume to close sampling and the sample introduction of pneumatic six-way valve Quality control, has realized the large-scale sample feeding of large volume, collection and preparation, has improved production efficiency;
2, the present invention adopts barrier film supercharging sampling technique, in the situation that sample quantitatively encircles given volume, has improved sample feeding amount, a certain amount of sample gas single efficiently can be transferred to sample and quantitatively encircle, and realizes the efficient sample introduction of sample;
3, the present invention's employing, to component desorption under high temperature in enriching column in conjunction with the method for barrier film supercharging diffusion transfer, has improved the efficiency that component shifts and collects;
4, the corresponding different gas of the present invention adopts the enriching column of different packing materials, has realized the independent enrichment of multiple goal component.
Accompanying drawing explanation
Fig. 1 is preparative gas chromatography working-flow schematic diagram of the present invention;
Fig. 2 is enriching column structural representation of the present invention;
Fig. 3 is that preparative gas chromatography system sample of the present invention quantitatively encircles sampling state work schematic diagram;
Fig. 4 is that preparative gas chromatography system sample of the present invention quantitatively encircles sample introduction state work schematic diagram;
Fig. 5 is that preparative gas chromatography system of the present invention forms schematic diagram;
Wherein: 1-carrier gas bottle; 2-gas filter; 3-sample source bottle; 4-pressure maintaining valve; 5-1-pressure gauge; 5-2-pressure gauge; 5-3-pressure gauge; 6-1-the-membrane pump; 6-2-the second membrane pump; The pneumatic six-way valve of 7-; 8-chromatographic column; 9-chromatographic detector; 10-enriching column and temperature regulating device thereof; 10-1-enriching column pipeline; 10-2-enriching column filler; 10-3-gas circuit connecting pipe; 11-component receiving flask; 12-cold-trap; 13-vacuum pump; 14-sample quantitatively encircles; V1～V8 and V10～V18 represent gas circuit stop valve; V9 represents three-way switch valve (original state is logical atmosphere).
Embodiment
The workflow of the preparative gas chromatography system that the present invention sets up as shown in Figure 1, comprises sample feeding, component is separated, component is collected, component shifts, component is concentrated and the step such as sample preparation.
The preparative gas chromatography system that the present invention sets up comprises gas sample introduction device, chromatographic resolution control device and component gathering-device, as shown in Figure 5.
Gas boosting sampling device comprises sample quantitatively ring 14, vacuum pump 13, membrane pump 6-1, pneumatic six-way valve 7, some valves and gas circuit pipe fitting, pneumatic six-way valve 7 comprises pneumatic six-way valve valve body and drives gas, drives gas to provide power for the switching of pneumatic six-way valve between sampling and sample introduction state; Membrane pump 6-1 realizes the mixed gas sample 1 quantitatively supercharging of ring 14 transfer from sample source bottle to sample, the quantitative ring 14 of sample and 7 couplings of pneumatic six-way valve realize sampling and the sample introduction of sample, vacuum pump 13 is for vacuumizing sampling device pipeline, at vacuum pump 13, sample, quantitatively encircle 14, be provided with valve between membrane pump 6-1 and pneumatic six-way valve 7, for the break-make of gas circuit, control; Sample of the present invention quantitatively encircles 14 bulk samples that adopt volumes to be not less than 12mL and quantitatively encircles, and by switching pneumatic six-way valve 7, makes sample quantitatively encircle 14 and be operated in respectively sampling and sample introduction state.As shown in Figure 3, when switching the switch of pneumatic six-way valve 7, while making that quantitatively the two ends of ring 14 connect respectively carrier gas 1 and mixed gas sample 3 through sample, sample quantitatively encircles 14 in sampling duty; As shown in Figure 4, when switching the switch of pneumatic six-way valve 7, make sample quantitatively connect respectively chromatographic column 8 in the two ends of ring 14, now sample quantitatively encircles 14 in sample introduction duty.When device designs in addition, reduce the quantitatively dead volume of pipeline between ring 14 of membrane pump 6-1 and sample as far as possible; Adopt membrane pump 6-1 the gaseous tension minimum in sample source bottle can be down to 100Pa left and right, membrane pump 6-1 top hole pressure maximum can reach approximately 5.0 * 10 simultaneously
5pa, thus the efficient sample introduction of sample gas can be guaranteed.
Gas chromatography separation control device comprises chromatogram main control system, chromatographic column 8, chromatographic detector 9, carrier gas 1 and connects gas circuit, carrier gas 1 quantitatively encircles sample in 14 by sample and is written into after chromatographic column 8, chromatographic detector 9 real-time parameters detect, and realize the chromatographic resolution of blending ingredients, chromatographic column 8 is 5
molecular sieve packed column, column internal diameter is 4mm, column length is 12m, chromatographic detector 9 is large volume thermal conductivity cell detector, can guarantee that the gas reserving from chromatographic column 8 all enters chromatographic detector 9 and can not affect the detection performance of chromatographic detector 9, gas composition is collected with preparation facilities and is comprised the enriching column 10 that many groups are in parallel, membrane pump 6-2, vacuum pump 13, component receiving flask 11, cold-trap 12, some valves and gas circuit pipe fitting, the gas of chromatographic detector 9 outputs enters respectively corresponding enriching column 10, enriching column 10 is held back for the absorption of sample component, after membrane pump 6-2, supercharging is transferred to component receiving flask 11, component receiving flask 11 is outside equipped with cold-trap 12, condensation separation for carrier gas and collection gas, vacuum pump 13 is for vacuumizing gathering-device pipeline, and for the eliminating of waste gas to realize the purifying of component.Between vacuum pump 13, chromatographic detector 9, membrane pump 6-2 and component receiving flask 11, be provided with valve, for the break-make of gas circuit, control.
The structure of enriching column 10 as shown in Figure 2, comprises enriching column pipeline 10-1 and gas circuit connecting pipe 10-3, is filled with enriching column filler 10-2 in enriching column pipeline 10-1, and every kind of enriching column filler 10-2 determines according to different gas.
Provided specific embodiment of the invention step below:
The gas chromatography separation and preparation of argon, krypton, xenon in certain biased sample gas is carried out in this experiment.In biased sample, the volume by volume concentration of argon, krypton, xenon is respectively 9.97%, 9.95% and 9.91%, and nitrogen is matrix gas.Sample is deposited in the stainless steel source bottle that volume is 36mL.
Specific experiment step is as follows:
(1) at the sample shown in Fig. 4, quantitatively encircle under 14 sampling states, by sample source bottle, by valve V1 access sampling device, maintenance source bottle carries valve closing;
(2) valve-off V2, V5 and V8, Open valve V1, V3, V4, V19 and V20, start vacuum pump 13, and the quantitative ring 14 of sample and associated pipe are evacuated to below 10Pa; (effect of V8 is exactly by a end sealing of pneumatic six-way valve, therefore always in closed condition.)
(3) valve-off V3 and V4; Cut off vacuum pump 13 power supplys, start membrane pump 6-1;
(4) open sample source bottle 3, sample gas is transferred to sample from the supercharging of sample source bottle and quantitatively encircles 14, the pressure of survival gas in pressure transducer 5-1 indication sample source bottle, the pressure of gas in simultaneously quantitatively encircling with pressure transducer 5-2 indication sample;
(5), after 5-1 pressure indication numerical value no longer changes, valve-off V20, cuts off membrane pump 6-1 power supply;
(6) guarantee chromatogram main frame and chromatographic detector 9 ready state in default chromatographic program, switch the pneumatic six-way valve 7 of startup and make the quantitatively ring 14 sample introduction states that are operated in as shown in Figure 4 of sample, carrier gas 1 quantitatively encircles sample in 14 by sample and is written into chromatographic column 8, complete the sample introduction of sample, and carry out the chromatographic resolution of blending ingredients;
(7) before target components flows out, guarantee that carrier gas 1 does not enter component receiving flask 11, valve V9 opens, and valve V10, V12 and V14 close;
(8), in above-mentioned default chromatographic program, the retention time of argon krypton xenon is respectively 4.3min, 5.6min and 10.9min; Argon krypton xenon chromatographic peak peak width is about respectively 1.0min, 2.0min and 5.0min.In each target components goes out the time period at peak, valve V9 is closed to corresponding enriching column 10 two ends valve opens, the i.e. corresponding V10 of argon and V11; The corresponding V12 of krypton and V13; The corresponding V14 of xenon and V15, and valve V16 opens, V17 closes;
(9) after treating the enrichment of xenon, guarantee all enriching column 10 two ends valve closings, valve V9 opens;
(10) according to the order of preparation target components to be transferred, the enriching column of this target components of enrichment 10 is heated to 280 ℃, and constant temperature 10min;
(11) take the transfer of target components in an enriching column is topmost example, starts membrane pump 6-2, and Open valve V11 and V17, be transferred to desorb component in enriching column 10 sample collection bottle 11 that is placed in cold-trap 12; After membrane pump 6-2 continuous firing 3min, valve-off V17, standing about 5min, makes target components fully cooling;
(12) Open valve V18 and V17, utilize uncooled carrier gas in system gas circuit, this enriching column of circulation flushing, the about 2min of continuous firing; Then valve-off V18, makes after the about 3min of membrane pump 6-2 continuous firing valve-off V17;
(13) close membrane pump 6-2, start vacuum pump 13, open valve V11, V10 and V18, the carrier gas in receiving flask 11 is emptying, during exhaust, be about 5s, then valve-off V18;
(14) receiving flask 11 is taken out from cold-trap 12, keep it to carry valve closing, change new source capsule, repeat (10)～(14) step, complete collection and the preparation of related component.
Claims (5)
1. a preparative gas chromatography system, comprises gas boosting sampling device, preparative gas chromatography separation control device, gas composition collection and preparation facilities and vacuum pump, it is characterized in that:
Described gas boosting sampling device comprises that sample quantitatively encircles, the first membrane pump, pneumatic six-way valve;
The import of described the first membrane pump communicates with sample source bottle by valve, and its outlet communicates with the b end of pneumatic six-way valve by valve; The described sample quantitatively two ends of ring communicates with f end and the c end of pneumatic six-way valve respectively; Described pneumatic six-way valve comprises pneumatic six-way valve valve body and drives gas, and described driving gas provides power for the switching of the pneumatic six-way valve of pneumatic six-way valve between sampling and sample introduction state;
Described preparative gas chromatography separation control device comprises chromatogram main control system, chromatographic column, chromatographic detector, carrier gas bottle; Described carrier gas bottle communicates with the e end of pneumatic six-way valve by valve; The import of described chromatographic column communicates with the d of pneumatic six-way valve end, and its outlet communicates with the entrance of chromatographic detector;
Described gas composition is collected with preparation facilities and is comprised enrichment unit, the second membrane pump, component receiving flask and the cold-trap with temperature regulating device; The entrance of described enrichment unit communicates with the outlet of chromatographic detector by valve, the outlet of described enrichment unit communicates with the entrance of the second membrane pump by valve, described the second barrier film delivery side of pump communicates with the entrance of component receiving flask in cold-trap, and the outlet of described component receiving flask communicates with the entrance of enrichment unit by valve;
The bleeding point of described vacuum pump by threeway after, the valve of leading up to communicates with sample source bottle and the first membrane pump entrance of gas boosting sampling device, the valve of separately leading up to communicates with outlet and the second membrane pump entrance of the enrichment unit (10) of preparation facilities with gas composition collection
Described enrichment unit is the enriching column of single enriching column or a plurality of parallel connections,
Described chromatographic column is 5
molecular sieve packed column, column internal diameter is 4mm, column length is 12m.
2. preparative gas chromatography system according to claim 1, is characterized in that: between described sample source bottle (3) and the first membrane pump (1), between the first membrane pump and the b end of pneumatic six-way valve (7), be respectively arranged with the pressure gauge of monitoring pipeline gaseous tension between chromatographic detector and enrichment unit.
3. preparative gas chromatography system according to claim 2, is characterized in that: described detecting device is large volume thermal conductivity cell detector; Described carrier gas is high pure nitrogen; Described enriching column filler is graininess cocoanut active charcoal, and granularity of activated carbon is 14～20 orders.
4. by the method for the separated inert gas sample of preparative gas chromatography system, it is characterized in that, comprise the following steps:
1] sample feeding:
1.1] access sample source bottle, keeps it to carry valve closing;
1.2] switch pneumatic six-way valve, make sample quantitatively encircle and be operated under sampling state, the quantitative ring of sample and auxiliary piping thereof are evacuated to below 10Pa;
1.3] open the valve that carries of sample source bottle, utilize membrane pump that sample gas is transferred to the quantitative ring of sample from sample source bottle;
1.4] switch pneumatic six-way valve, sample is quantitatively encircled in sample introduction state;
1.5] utilize carrier gas will quantitatively encircle in sample be written into chromatographic column, the pressure during simultaneously with pressure gauge indication sample introduction, described chromatographic column is 5
molecular sieve packed column, column internal diameter is 4mm, column length is 12m;
2] component separation and enrichment:
2.1] adopt the calibrating gas of target components, determine optimization chromatographic condition and the sensors work parameter of component separation, set up chromatographic applications program;
2.2], in the chromatographic applications program of setting up, determine the chromatographic retention of each target components;
2.3] start chromatographic applications program, according to the retention time of fixed each component, control the three-way switch valve of detecting device rear end, target components is switched to corresponding enriching column and carries out enrichment;
3] component desorb:
After component enrichment finishes, enriching column is heated to be not less than 200 ℃ under closed state, and constant temperature 10min, make target components desorb completely from enriching column;
4] component shifts:
Adopt membrane pump, desorb component in enriching column is transferred in component receiving flask, open the circulation gas circuit between receiving flask and enriching column, rinse enriching column;
5] component rectifying and sample preparation:
5.1] by cold-trap, the temperature of component receiving flask is down to below the boiling point of target components, makes target components completely in condensing state;
5.2] unlatching vacuum pump is emptying by the residual gas component in sample source bottle, the concentrated collection of realize target component.
5. the method with the separated inert gas sample of preparative gas chromatography system according to claim 4, is characterized in that: described detecting device is large volume thermal conductivity cell detector; Described carrier gas is high pure nitrogen; Described enriching column is active carbon filler enriching column.
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| CN105344203A (en) * | 2015-12-02 | 2016-02-24 | 衢州铭泰仪器设计有限公司 | Gas separation device and method for gas separation by utilizing device |
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| CN108490092A (en) * | 2018-03-27 | 2018-09-04 | 天津大学 | A kind of gas detecting system |
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| CN113272644B (en) * | 2019-02-19 | 2024-01-12 | 株式会社岛津制作所 | Gas separation system |
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| JP7226223B2 (en) * | 2019-09-24 | 2023-02-21 | 株式会社島津製作所 | gas sampler |
| CN115219639A (en) * | 2021-04-15 | 2022-10-21 | 中国石油天然气股份有限公司 | System for enriching hydrocarbon gas in slurry gas and using method thereof |
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