CN102323359A - 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 the method that a kind of gas chromatography piece-rate system and gas chromatography piece-rate system are used to separate the inert gas sample, particularly a kind of method for preparing the type gas chromatography system and prepare the inert gas sample.
Background technology
Gas chromatography is a kind of analysis means of routine, on application purpose, roughly is divided into analytic type gas chromatography and preparation type gas chromatography two big classes, 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 significant difference is arranged also; The analytic type chromatogram requires less sample introduction or trace sample introduction, helps forming symmetrical chromatographic peak, reduces hangover; Preparative scale chromatography then is under the prerequisite of product purity that guarantees to reach certain and yield, requires to improve the sample size and the product volume of chromatographic column.The principal element of the type of restriction preparation at present gas chromatographic technique development is to be difficult to realize the large-scale sample feeding of big volume, collection and preparation, causes production efficiency lower.
Summary of the invention
The object of the invention provides a kind of method for preparing the type gas chromatography system and separate the inert gas sample; It has solved the technical matters that is difficult to realize the large-scale sample feeding of big volume, collection and preparation that exists in existing gas chromatography system and the application thereof, has improved production efficiency.
Technical solution of the present invention is:
A kind of preparation type gas chromatography system; Comprise gas boosting sampling device, preparation gas chromatography separation control device, gas composition collection and preparation facilities and vacuum pump, its special character is: said gas boosting sampling device comprises sample quantifying ring, first membrane pump, pneumatic six-way valve; The import of said first membrane pump communicates with the sample source bottle through valve, and its outlet communicates with the b end of pneumatic six-way valve through valve; The two ends of said sample quantifying ring communicate with the f end and the c end of pneumatic six-way valve respectively; Said pneumatic six-way valve comprises pneumatic six-way valve valve body and drives gas that said driving gas is that the switching of the pneumatic six-way valve of pneumatic six-way valve between sample circuit sample introduction state provides power; Said preparation gas chromatography separation control device comprises chromatogram main control system, chromatographic column, chromatographic detector, carrier gas bottle; Said carrier gas bottle communicates with the e end of pneumatic six-way valve through valve; The import of said chromatographic column communicates with the d of pneumatic six-way valve end, and its outlet communicates with the inlet of chromatographic detector; Said gas composition is collected with preparation facilities and is comprised enrichment unit, second membrane pump, component receiving flask and the cold-trap that has temperature regulating device; The inlet of said enrichment unit communicates with the outlet of chromatographic detector through valve; The outlet of said enrichment unit communicates through the inlet of valve with second membrane pump; The inlet of the component receiving flask in the said second barrier film delivery side of pump and the cold-trap communicates, and the outlet of said component receiving flask communicates through the inlet of valve with the enrichment unit; The bleeding point of said vacuum pump through threeway after; The valve of leading up to communicates with the sample source bottle and first membrane pump inlet of gas boosting sampling device, and another road communicates with the outlet and second membrane pump inlet of the enrichment unit 10 of preparation facilities through valve and gas composition collection.
Between the above-mentioned sample source bottle 3 and first membrane pump 1, between the b end of first membrane pump and pneumatic six-way valve 7, be respectively arranged with the pressure gauge of monitoring pipeline gaseous tension between chromatographic detector and the enrichment unit.
Above-mentioned enrichment unit is the enriching column of single enriching column or a plurality of parallel connections.
Above-mentioned chromatographic column be 5
molecular sieve packed column; Column internal diameter is 4mm, and column length is 12m; Above-mentioned detecting device is big volume thermal conductivity cell detector; Above-mentioned carrier gas is a high pure nitrogen; Above-mentioned enriching column filler is the graininess cocoanut active charcoal, and granularity of activated carbon is 14~20 orders.
With the above-mentioned method for preparing type gas chromatography system separation inert gas sample, may further comprise the steps:
1] sample feeding:
1.1] insert the sample source bottle, keep it to carry valve closing;
1.2] switch pneumatic six-way valve, make the sample quantifying ring be operated under the sample, sample quantifying ring and auxiliary piping thereof are evacuated to below the 10Pa;
1.3] open the valve that carries of sample source bottle, utilize membrane pump that sample gas is transferred to the sample quantifying ring from the sample source bottle;
1.4] switch pneumatic six-way valve, make the sample quantifying ring be in the sample introduction state;
1.5] utilize carrier gas that sample in the quantifying ring is written into chromatographic column, the pressure during simultaneously with pressure gauge indication sample introduction;
2] component is separated and enrichment:
2.1] adopt the calibrating gas of target components, confirm optimization chromatographic condition and sensors work parameter that component is separated, set up the chromatographic applications program;
2.2] in the chromatographic applications program of setting up, confirm the chromatographic retention of each target components;
2.3] start the chromatographic applications program, according to the retention time of fixed each component, the three-way switch valve of control detection device rear end is cut target group to corresponding enriching column and is carried out enrichment;
3] component desorb:
After the component enrichment finishes, enriching column is heated under closed state is not less than 200 ℃, and constant temperature 10min, make target components desorb fully from enriching column;
4] component shifts:
Adopt membrane pump, desorb component in the enriching column is transferred in the component receiving flask, open the circulation gas circuit between receiving flask and the enriching column, the flushing enriching column;
5] component rectifying and specimen preparation:
5.1] through cold-trap the temperature of component receiving flask is reduced to below the boiling point of target components, make target components be in condensing state fully;
5.2] the open vacuum pump is the residual gas component emptying in the sample source bottle, realizes the concentrated collection of target components.
Above-mentioned chromatographic column be 5
molecular sieve packed column; Column internal diameter is 4mm, and column length is 12m; Above-mentioned detecting device is big volume thermal conductivity cell detector; Above-mentioned carrier gas is a high pure nitrogen; Above-mentioned enriching column is the active carbon filler enriching column.
The beneficial effect that the present invention has:
1, the present invention adopts the sample quantifying ring of big volume to combine the sample circuit sample introduction of pneumatic six-way valve control sample, has realized the large-scale sample feeding of big volume, collection and preparation, has improved production efficiency;
2, the present invention adopts barrier film supercharging sampling technique, under the situation of sample quantifying ring given volume, has improved the sample feeding amount, can quantity of sample gas single efficiently be transferred to the sample quantifying ring, realizes the efficient sample introduction of sample;
3, the present invention adopts the method that component high temperature desorb in the enriching column is combined barrier film supercharging diffusion transfer, has improved the efficient 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.
Description of drawings
Fig. 1 prepares type gas chromatography system workflow synoptic diagram for the present invention;
Fig. 2 is an enriching column structural representation of the present invention;
Fig. 3 prepares type gas chromatography system sample quantifying ring sample work synoptic diagram for the present invention;
Fig. 4 prepares type gas chromatography system sample quantifying ring sample introduction state work synoptic diagram for the present invention;
Fig. 5 forms synoptic diagram for the present invention prepares the type gas chromatography system;
Wherein: the 1-carrier gas bottle; The 2-gas filter; 3-sample source bottle; The 4-pressure maintaining valve; The 5-1-pressure gauge; The 5-2-pressure gauge; The 5-3-pressure gauge; 6-1-the-membrane pump; 6-2-second membrane pump; The pneumatic six-way valve of 7-; The 8-chromatographic column; The 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; The 12-cold-trap; The 13-vacuum pump; 14-sample quantifying ring; V1~V8 and V10~V18 represent the gas circuit stop valve; V9 representes three-way switch valve (original state is logical atmosphere).
Embodiment
The workflow of the preparation gas chromatography system that the present invention sets up is as shown in Figure 1, comprises that sample feeding, component are separated, component is collected, component shifts, component concentrates and step such as specimen preparation.
The preparation type gas chromatography system that the present invention sets up comprises gas sample introduction device, chromatographic resolution control device and component gathering-device, and is as shown in Figure 5.
The gas boosting sampling device comprises sample quantifying ring 14, vacuum pump 13, membrane pump 6-1, pneumatic six-way valve 7, the gentle road of some valves pipe fitting; Pneumatic six-way valve 7 comprises pneumatic six-way valve valve body and drives gas that driving gas is that the switching of pneumatic six-way valve between sample circuit sample introduction state provides power; Membrane pump 6-1 realizes that mixed gas sample 1 supercharging from the sample source bottle to sample quantifying ring 14 shifts; The sample circuit sample introduction of sample quantifying ring 14 and pneumatic six-way valve 7 couplings realization sample; Vacuum pump 13 is used for the sampling device pipeline is vacuumized; Between vacuum pump 13, sample quantifying ring 14, membrane pump 6-1 and pneumatic six-way valve 7, be provided with valve, be used for the break-make control of gas circuit; Sample quantifying ring 14 of the present invention adopts volume to be not less than the bulk sample quantifying ring of 12mL, and through switching pneumatic six-way valve 7, makes sample quantifying ring 14 be operated in sample circuit sample introduction state respectively.As shown in Figure 3, when the switch that switches pneumatic six-way valve 7, when feasible two ends through sample quantifying ring 14 connected carrier gas 1 with mixed gas sample 3 respectively, sample quantifying ring 14 was in the sampling duty; As shown in Figure 4, the switch when switching pneumatic six-way valve 7 makes the two ends of sample quantifying ring 14 connect chromatographic column 8 respectively, and sample quantifying ring 14 is in the sample introduction duty at this moment.Reduce the dead volume of pipeline between membrane pump 6-1 and the sample quantifying ring 14 when device designs in addition as far as possible; Adopt membrane pump 6-1 can the gaseous tension minimum in the sample source bottle be reduced to about 100Pa simultaneously, membrane pump 6-1 top hole pressure maximum can reach about 5.0 * 10
5Pa, thus the efficient sample introduction of sample gas can be guaranteed.
The 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 is with after sample is written into chromatographic column 8 in the sample quantifying ring 14; Chromatographic detector 9 real-time parameters detect, and realize the chromatographic resolution of blending ingredients; Chromatographic column 8 be 5
molecular sieve packed column; Column internal diameter is 4mm, and column length is 12m; Chromatographic detector 9 is big volume thermal conductivity cell detector, can guarantee all to get into chromatographic detector 9 from the gas that chromatographic column 8 is reserved and can not influence the detection performance of chromatographic detector 9; Gas composition is collected with preparation facilities and is comprised parallelly connected enriching column 10, membrane pump 6-2, vacuum pump 13, component receiving flask 11, cold-trap 12, the gentle road of the some valves pipe fitting of many groups; The gas of chromatographic detector 9 outputs gets into corresponding enriching column 10 respectively; Enriching column 10 is used for the absorption of sample component and holds back; Be transferred to component receiving flask 11 through supercharging behind the membrane pump 6-2, component receiving flask 11 is outside equipped with cold-trap 12, is used for carrier gas and the condensation separation of collecting gas; Vacuum pump 13 is used for the gathering-device pipeline is vacuumized, and is used for the purifying of the eliminating of waste gas with the realization component.Between vacuum pump 13, chromatographic detector 9, membrane pump 6-2 and component receiving flask 11, be provided with valve, be used for the break-make control of gas circuit.
The structure of enriching column 10 is as shown in Figure 2, comprises the gentle connecting pipe 10-3 of enriching column pipeline 10-1, in enriching column pipeline 10-1, is filled with enriching column filler 10-2, and every kind of enriching column filler 10-2 decides according to different gas.
Provided practical implementation step of the present invention below:
This experiment is carried out the gas chromatography of argon, krypton, xenon in certain biased sample gas and is separated and preparation.The volume by volume concentration of argon, krypton, xenon is respectively 9.97%, 9.95% and 9.91% in the biased sample, and nitrogen is matrix gas.Sample is deposited in the stainless steel source bottle that volume is 36mL.
Concrete experimental procedure is following:
(1) under sample quantifying ring 14 sample shown in Figure 4, the sample source bottle is inserted sampling device through valve V1, 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 sample quantifying ring 14 and associated pipe are evacuated to below the 10Pa; (effect of V8 is exactly a end sealing with pneumatic six-way valve, so be in closed condition always.)
(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 the sample quantifying ring 14 from the supercharging of sample source bottle, pressure transducer 5-1 indicates the pressure of survival gas in the sample source bottle, indicates the pressure of gas in the sample quantifying ring simultaneously with pressure transducer 5-2;
(5) treat that 5-1 pressure indication numerical value no longer changes after, valve-off V20 cuts off membrane pump 6-1 power supply;
(6) guarantee that chromatogram main frame and chromatographic detector 9 are in the ready state of preset chromatographic program; Switching the pneumatic six-way valve 7 of startup makes sample quantifying ring 14 be operated in sample introduction state as shown in Figure 4; Carrier gas 1 is written into chromatographic column 8 with sample in the sample quantifying ring 14; Accomplish 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 get into component receiving flask 11, promptly valve V9 opens, and valve V10, V12 and V14 close;
(8) in above-mentioned preset 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 1.0min, 2.0min and 5.0min respectively.In each target group was told the time period at peak, V9 closed with valve, corresponding enriching column 10 two ends valve opens, i.e. corresponding V10 of argon and V11; Corresponding V12 of krypton and V13; Corresponding V14 of xenon and V15, and valve V16 opens, V17 closes;
(9) after the enrichment of treating xenon finishes, 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 10 of this target components of enrichment is heated to 280 ℃, and constant temperature 10min;
(11) transfer with target components in the enriching column in the top is an example, starts membrane pump 6-2, and Open valve V11 and V17 are transferred to desorb component in the enriching column 10 sample collection bottle 11 that places cold-trap 12; Behind the membrane pump 6-2 continuous firing 3min, valve-off V17 leaves standstill about 5min, and target components is fully cooled off;
(12) Open valve V18 and V17 utilize uncooled carrier gas in system's gas circuit, this enriching column of circulation flushing, the about 2min of continuous firing; Valve-off V18 then, make the about 3min of membrane pump 6-2 continuous firing after, valve-off V17;
(13) close membrane pump 6-2, start vacuum pump 13, open valve V11, V10 and V18, the carrier gas emptying with in the receiving flask 11 is about 5s during exhaust, 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, accomplish the collection and the preparation of related component.
Claims (6)
1. one kind prepares the type gas chromatography system, comprises gas boosting sampling device, preparation gas chromatography separation control device, gas composition collection and preparation facilities and vacuum pump, it is characterized in that:
Said gas boosting sampling device comprises sample quantifying ring, first membrane pump, pneumatic six-way valve;
The import of said first membrane pump communicates with the sample source bottle through valve, and its outlet communicates with the b end of pneumatic six-way valve through valve; The two ends of said sample quantifying ring communicate with the f end and the c end of pneumatic six-way valve respectively; Said pneumatic six-way valve comprises pneumatic six-way valve valve body and drives gas that said driving gas is that the switching of the pneumatic six-way valve of pneumatic six-way valve between sample circuit sample introduction state provides power;
Said preparation gas chromatography separation control device comprises chromatogram main control system, chromatographic column, chromatographic detector, carrier gas bottle; Said carrier gas bottle communicates with the e end of pneumatic six-way valve through valve; The import of said chromatographic column communicates with the d of pneumatic six-way valve end, and its outlet communicates with the inlet of chromatographic detector;
Said gas composition is collected with preparation facilities and is comprised enrichment unit, second membrane pump, component receiving flask and the cold-trap that has temperature regulating device; The inlet of said enrichment unit communicates with the outlet of chromatographic detector through valve; The outlet of said enrichment unit communicates through the inlet of valve with second membrane pump; The inlet of the component receiving flask in the said second barrier film delivery side of pump and the cold-trap communicates, and the outlet of said component receiving flask communicates through the inlet of valve with the enrichment unit;
The bleeding point of said vacuum pump through threeway after; The valve of leading up to communicates with the sample source bottle and first membrane pump inlet of gas boosting sampling device, and another road communicates with the outlet and second membrane pump inlet of the enrichment unit 10 of preparation facilities through valve and gas composition collection.
2. preparation type gas chromatography system according to claim 1 is characterized in that: between the said sample source bottle 3 and first membrane pump 1, between the b end of first membrane pump and pneumatic six-way valve 7, be respectively arranged with the pressure gauge of monitoring pipeline gaseous tension between chromatographic detector and the enrichment unit.
3. preparation type gas chromatography system according to claim 1 and 2 is characterized in that: said enrichment unit is the enriching column of single enriching column or a plurality of parallel connections.
4. preparation type gas chromatography system according to claim 3; It is characterized in that: described chromatographic column be 5
molecular sieve packed column; Column internal diameter is 4mm, and column length is 12m; Described detecting device is big volume thermal conductivity cell detector; Described carrier gas is a high pure nitrogen; Described enriching column filler is the graininess cocoanut active charcoal, and granularity of activated carbon is 14~20 orders.
5. with preparing the method that the type gas chromatography system separates the inert gas sample, it is characterized in that, may further comprise the steps:
1] sample feeding:
1.1] insert the sample source bottle, keep it to carry valve closing;
1.2] switch pneumatic six-way valve, make the sample quantifying ring be operated under the sample, sample quantifying ring and auxiliary piping thereof are evacuated to below the 10Pa;
1.3] open the valve that carries of sample source bottle, utilize membrane pump that sample gas is transferred to the sample quantifying ring from the sample source bottle;
1.4] switch pneumatic six-way valve, make the sample quantifying ring be in the sample introduction state;
1.5] utilize carrier gas that sample in the quantifying ring is written into chromatographic column, the pressure during simultaneously with pressure gauge indication sample introduction;
2] component is separated and enrichment:
2.1] adopt the calibrating gas of target components, confirm optimization chromatographic condition and sensors work parameter that component is separated, set up the chromatographic applications program;
2.2] in the chromatographic applications program of setting up, confirm the chromatographic retention of each target components;
2.3] start the chromatographic applications program, according to the retention time of fixed each component, the three-way switch valve of control detection device rear end is cut target group to corresponding enriching column and is carried out enrichment;
3] component desorb:
After the component enrichment finishes, enriching column is heated under closed state is not less than 200 ℃, and constant temperature 10min, make target components desorb fully from enriching column;
4] component shifts:
Adopt membrane pump, desorb component in the enriching column is transferred in the component receiving flask, open the circulation gas circuit between receiving flask and the enriching column, the flushing enriching column;
5] component rectifying and specimen preparation:
5.1] through cold-trap the temperature of component receiving flask is reduced to below the boiling point of target components, make target components be in condensing state fully;
5.2] the open vacuum pump is the residual gas component emptying in the sample source bottle, realizes the concentrated collection of target components.
6. according to claim 5 with preparing the method that the type gas chromatography system separates the inert gas sample; It is characterized in that: described chromatographic column be 5
molecular sieve packed column; Column internal diameter is 4mm, and column length is 12m; Described detecting device is big volume thermal conductivity cell detector; Described carrier gas is a high pure nitrogen; Described enriching column is the active carbon filler enriching column.
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CN103033568A (en) * | 2011-09-29 | 2013-04-10 | 中国石油化工股份有限公司 | Quick chromatographic analysis method for trace ammonia in gas |
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CN107884481A (en) * | 2016-09-30 | 2018-04-06 | 中国石油化工股份有限公司 | For determining the detecting system and detection method of weight rare gas content in natural gas |
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CN108732287A (en) * | 2018-08-08 | 2018-11-02 | 成都科林分析技术有限公司 | A kind of thermal desorption gas sample injection device and method |
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CN110161139A (en) * | 2019-05-23 | 2019-08-23 | 中国辐射防护研究院 | A kind of large volume non-quantitative sample injection method using gas chromatograph separation Kr-85 |
US20210088484A1 (en) * | 2019-09-24 | 2021-03-25 | Shimadzu Corporation | Gas sampler |
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