CN106706831A - Multifunctional on-line gas preparation and introduction system cold trap preenrichment device - Google Patents
Multifunctional on-line gas preparation and introduction system cold trap preenrichment device Download PDFInfo
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- CN106706831A CN106706831A CN201710089645.0A CN201710089645A CN106706831A CN 106706831 A CN106706831 A CN 106706831A CN 201710089645 A CN201710089645 A CN 201710089645A CN 106706831 A CN106706831 A CN 106706831A
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- trap
- cold
- gas
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- cold trap
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- 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
-
- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
-
- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8804—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 automated systems
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a multifunctional on-line gas preparation and introduction system cold trap preenrichment device, and relates to analysis testing techniques. The multifunctional on-line gas preparation and introduction system cold trap preenrichment device comprises a sample bottle, a first drying tube, a magnesium perchlorate tube, an eight-way valve, a first liquid nitrogen tank, a first cold trap, a first pneumatic rod, a second liquid nitrogen tank, a second cold trap, a second pneumatic rod, a chromatographic column, a second drying tube and a mass spectrometer, wherein a blowing sample gas is fed into the sample bottle through a bidirectional sample feeding needle; the sample gas which flows out from the sample bottle through the bidirectional sample feeding needle is fed into the first cold trap through the eight-way valve after sequentially passing through the first drying tube and the magnesium perchlorate tube; the sample gas is enriched by the first cold trap and is discharged out from the eight-way valve; a He gas passes through the eight-way valve and is fed into the mass spectrometer from the second cold trap, the chromatographic column and the second drying tube in sequence, and thus detection on the sample gas can be completed; the first cold trap is arranged inside the first liquid nitrogen tank; the first pneumatic rod is connected with the first cold trap; the second cold trap is arranged in the second liquid nitrogen tank; the second pneumatic rod is connected with the second cold trap.
Description
Technical field
The present invention relates to analysis and testing technology, prepared and the pre- richness of import system cold-trap more particularly, to the online gas of multipurpose
Acquisition means.
Background technology
Headspace sampling technology is a kind of easily and efficiently sample-pretreating method in gas chromatography.Its principle is to treat
Test sample product are inserted in a closed container, heated up by physical heating or chemical method makes volatile component be waved from sample matrices
Issue, balance is reached in gas-liquid (or gas-solid) two-phase, directly extracting top gas carries out chromatography.Headspace gas chromatography
Method will only volatilize and the component of half volatilization introduces chromatographic column, can be prevented effectively from the serious dirt that non-volatile material is caused to system
Dye, simple and convenient sample treatment, analysis efficiency is high.The online gas of multipurpose of Thermo Scientific is prepared and import system
Headspace sampling equipment is more universal headspace sampling device, can be used in conjunction with corresponding isotope ratio mass spectrometer, analysis test water
The gaseous component generated after the samples such as hydrogen, oxygen, carbon dioxide, the nitrogen of dissolving of body and the acidifying of solid carbonic acid salt material,
Be automation, the headspace sampling system of efficiently and accurately, the micro object gas extremely low for the relative concentration in gaseous sample, such as
The gas such as methane, nitrous oxide and carbon dioxide in air, micro object gas during conventional headspace sampling in quantitative loop are not enough
The signal intensity of analysis is met to produce, so needing to carry out preenrichment to meet analysis demand by cold-trap.
The content of the invention
Prepared and import system present invention aim at a kind of online gas of multipurpose based on liquid nitrogen trapping principle is provided
Cold-trap preenrichment device.
The present invention is provided with sample bottle, the 1st drying tube, magnesium perchlorate pipe, eight ways valve, the 1st liquid nitrogen container, the 1st cold-trap, the 1st gas
Dynamic rod, the 2nd liquid nitrogen container, the 2nd cold-trap, the 2nd pneumatic rod, chromatographic column, the 2nd drying tube and mass spectrograph；Purging sample gas through it is two-way enter
Sample pin enters sample bottle, and the 1st drying tube and magnesium perchlorate are passed sequentially through by the sample gas that two-way sample introduction needle flows out by sample bottle
Guan Hou, through eight ways valve enter the 1st cold-trap, through the 1st cold-trap enriched sample gas through eight ways valve discharge, He gas by after eight ways valve successively
Enter mass spectrograph through the 2nd cold-trap, chromatographic column and the 2nd drying tube, complete the detection of sample gas；1st cold-trap is located at the 1st liquid nitrogen
In tank, the 1st pneumatic rod is connected with the 1st cold-trap, and in the 2nd liquid nitrogen container, the 2nd pneumatic rod is connected the 2nd cold-trap with the 2nd cold-trap.
1st cold-trap can be fixed on sheet metal using joint, and sheet metal is fixed on the 1st pneumatic rod top and with the 1st
Pneumatic rod lifting, the joint can use bulkhead adaptor.
2nd liquid nitrogen container can be fixed on sheet metal using joint, and sheet metal is fixed on the 2nd cold-trap top and with the 2nd
Cold-trap is lifted, and the joint can use bulkhead adaptor.
The present invention is prepared by the online gas of existing Thermo Scientific multipurposes and import system gas circuit changes
Make, increase chemical trap, water removal trap and two liquid nitrogen trapping cold-traps, and carried out modularization change, can meet to extremely low concentration
The requirement of object analysis.Liquid nitrogen cold trap prepares what the pneumatic operated valve reserved with import system was controlled using by the online gas of multipurpose
Pneumatic rod controls the lifting of cold-trap, at the same in order to after preventing cold-trap from being risen from liquid nitrogen stainless steel tube temperature it is too low, object gas
Chemical combination can not gasify, and heater strip is specially wrapped up on the outside of high speed cold-trap to lift cold-trap programming rate.Due to the liter of liquid nitrogen cold trap
Drop realizes software control, coordinates the online gas of multipurpose to prepare and is realized to high-volume low concentration intentional gas with import system
Chemical combination automatically analyzes test.
The present invention includes modular chemical trap and containing two cold-trap preenrichment apparatus main bodies of cold-trap, wherein the
1 cold-trap is made up of a stainless steel tube for being about 2m (1/16 "), includes the nickel wire (diameter that two same length are twisted into twisted shape
0.25mm).Nickel wire act as：1st, N is promoted2The freezing enrichment of O；2nd, remaining CO is prevented2Ice pellets is frozen into steam block stainless steel
Pipe.2nd cold-trap is a stainless steel capillary for being about 2m (external diameter 0.5mm, internal diameter 0.3mm).Cold-trap is solid with bulkhead adaptor
It is scheduled on sheet metal, sheet metal is fixed on air pressure rod top, with its lifting.The two ends of cold-trap are the stainless of 0.5mm with external diameter
Steel wool tubule is connected with Gasbench：1st cold-trap two ends are connected with two-way eight ways valve；The end of 2nd cold-trap one is connected in eight ways valve, separately
One end is connected to chromatographic column sample introduction end.1st cold-trap is used to be enriched with the trace gas that He gas under high flow condition is purged out from liquid
Body；The 2nd cold-trap minimum gas that further the 1st cold-trap of concentration has been enriched with, and chromatographic column is passed at low flow rates
(PoraPlotQ, Agilent) is isolated and purified.
Compared with prior art, the present invention has advantages below：
(1) using modular chemical trap composition, different trace gas analysis demands are met；
(2) gasification of object gas compound in liquid nitrogen cold trap is increased by heater strip；
(3) the individually separable characteristic of each several part makes cold-trap preenrichment device realize the characteristics of easily repairing, and then is lifted
The durability of whole device；
(4) material simple and easy to get is used, the cost for using can be safeguarded with lowering apparatus.
(5) the automated analysis test that Multi-example is realized with gatherer is prepared with reference to the online gas of multipurpose.
Brief description of the drawings
Fig. 1 is the structure composition schematic diagram of the embodiment of the present invention.
Fig. 2 is the purge and trap pattern gas circuit of the embodiment of the present invention.
Fig. 3 is the sample introduction analytical model gas circuit of the embodiment of the present invention.
Specific embodiment
Below by way of specific embodiment, the invention will be further described.
Referring to Fig. 1~3, the embodiment of the present invention is provided with sample bottle 1, the 1st drying tube 2, magnesium perchlorate pipe 3, eight ways valve the 4, the 1st
Liquid nitrogen container 5, the 1st cold-trap 6, the 1st pneumatic rod 7, the 2nd liquid nitrogen container 8, the 2nd cold-trap 9, the 2nd pneumatic rod 10, chromatographic column the 11, the 2nd are dried
Pipe 12 and mass spectrograph 13；Purging sample gas enter sample bottle 1 through two-way sample introduction needle A, are flowed by two-way sample introduction needle A by sample bottle 1
After the sample gas for going out pass sequentially through the 1st drying tube 2 and magnesium perchlorate pipe 3, enter the 1st cold-trap 6 through eight ways valve 4, through the 1st cold-trap 6
Enriched sample gas is discharged through eight ways valve 4, He gas by after eight ways valve 4 successively through the 2nd cold-trap 9, the drying tube 12 of chromatographic column 11 and the 2nd
Into mass spectrograph 13, the detection of sample gas is completed；1st cold-trap 6 is in the 1st liquid nitrogen container 5, and the 1st pneumatic rod 7 is cold with the 1st
Trap 6 is connected, and in the 2nd liquid nitrogen container 8, the 2nd pneumatic rod 10 is connected the 2nd cold-trap 9 with the 2nd cold-trap 9.
1st cold-trap 6 is fixed on sheet metal using joint, and sheet metal is fixed on the top of the 1st pneumatic rod 7 and with the 1st
Pneumatic rod 7 is lifted, and the joint uses bulkhead adaptor.
2nd liquid nitrogen container 8 is fixed on sheet metal using joint, and sheet metal is fixed on the top of the 2nd cold-trap 9 and with the 2nd
Cold-trap 9 is lifted, and the joint uses bulkhead adaptor.
The sample gas that the present invention will be purged out first are removed water by Nafion drying tubes, magnesium perchlorate and alkali soda removes two
The chemical trap of the modularization of carbonoxide etc. carries out the removal of foreign gas and moisture, is filled with nickel by immersion liquid nitrogen afterwards
The stainless steel tube of silk carries out the first step enrichment under high velocity air, while this cold-trap also has remove water function concurrently, preliminary concentration afterwards
Sample gas afterwards are enriched with by the second step for carrying out low speed flow by stainless steel capillary immersed in liquid nitrogen again.By rich twice
After collection, minimum gas are sufficient for the requirement needed for analyzing.(1) purge and trap pattern：High-purity He is passed through with the flow velocity of 25ml/min
Cross the stainless steel that external diameter is 0.75mm to enter in sample vial, as lighter He gas gathers at the top of sample bottle, gradually reduce
Sample in sample bottle flows out sample bottle by STH sample introduction needle, and then is the capillary or uniform internal diameter of 0.3mm by internal diameter
Stainless steel capillary, through remove water trap, except CO2Chemical trap, eight ways valve and the enrichment of first liquid nitrogen cold trap after, other other rows
It is empty.(2) test pattern is analyzed：Switching eight ways valve, high-purity He passes through eight ways valve with the flow rate of carrier gas of 3ml/min, into first
Liquid nitrogen cold trap (cold-trap departs from liquid nitrogen, the release of target compound gas), carrier gas carries target compound second cold-trap richness of gas
Collection (in second cold-trap immersion liquid nitrogen), second cold-trap rises after 10min, while cold-trap is heated, object gas compound, then
Mass spectrum is segregated into by chromatographic column, the detection of object gas is completed.
The present invention realizes the modularization of highly integrated original-pack cold-trap preenrichment device using pneumatic rod and liquid nitrogen cold trap
Reproduce, the online gas of multipurpose is prepared and improves system with the replaceability of each several part of import system cold-trap preenrichment device
The convenience of assembling, reduces maintenance maintenance difficulty, realizes economical and practical reliable and stable job requirement, exists with reference to multipurpose
Prepared by line gas and import system is realized automatically analyzing test to low concentration intentional gaseous compound isotope.
Claims (5)
1. the online gas of multipurpose is prepared and import system cold-trap preenrichment device, it is characterised in that be provided with sample bottle, the 1st drying
Pipe, magnesium perchlorate pipe, eight ways valve, the 1st liquid nitrogen container, the 1st cold-trap, the 1st pneumatic rod, the 2nd liquid nitrogen container, the 2nd cold-trap, the 2nd pneumatic rod,
Chromatographic column, the 2nd drying tube and mass spectrograph；Purging sample gas enter sample bottle through two-way sample introduction needle, by sample bottle by it is two-way enter
After the sample gas of sample pin outflow pass sequentially through the 1st drying tube and magnesium perchlorate pipe, enter the 1st cold-trap through eight ways valve, through the 1st cold-trap
Enriched sample gas is discharged through eight ways valve, and He gas through the 2nd cold-trap, chromatographic column and the 2nd drying tube by entering matter successively after eight ways valve
Spectrometer, completes the detection of sample gas；In the 1st liquid nitrogen container, the 1st pneumatic rod is connected 1st cold-trap with the 1st cold-trap, and the 2nd is cold
In the 2nd liquid nitrogen container, the 2nd pneumatic rod is connected trap with the 2nd cold-trap.
2. the online gas of multipurpose as claimed in claim 1 is prepared and import system cold-trap preenrichment device, it is characterised in that institute
State the 1st cold-trap to be fixed on sheet metal using joint, sheet metal is fixed on the 1st pneumatic rod top and is lifted with the 1st pneumatic rod.
3. the online gas of multipurpose as claimed in claim 3 is prepared and import system cold-trap preenrichment device, it is characterised in that institute
State joint and use bulkhead adaptor.
4. the online gas of multipurpose as claimed in claim 1 is prepared and import system cold-trap preenrichment device, it is characterised in that institute
State the 2nd liquid nitrogen container to be fixed on sheet metal using joint, sheet metal is fixed on the 2nd cold-trap top and is lifted with the 2nd cold-trap.
5. the online gas of multipurpose as claimed in claim 4 is prepared and import system cold-trap preenrichment device, it is characterised in that institute
State joint and use bulkhead adaptor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710089645.0A CN106706831A (en) | 2017-02-20 | 2017-02-20 | Multifunctional on-line gas preparation and introduction system cold trap preenrichment device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710089645.0A CN106706831A (en) | 2017-02-20 | 2017-02-20 | Multifunctional on-line gas preparation and introduction system cold trap preenrichment device |
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| CN106706831A true CN106706831A (en) | 2017-05-24 |
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| CN201710089645.0A Pending CN106706831A (en) | 2017-02-20 | 2017-02-20 | Multifunctional on-line gas preparation and introduction system cold trap preenrichment device |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107328846A (en) * | 2017-08-10 | 2017-11-07 | 中国科学院长春应用化学研究所 | Mass spectrum sampling system and cooling device |
| CN107941891A (en) * | 2017-10-12 | 2018-04-20 | 中国石油天然气股份有限公司 | A kind of method of C-O isotopes in on-line period measure microcell carbonate |
| CN110095575A (en) * | 2019-05-08 | 2019-08-06 | 中国科学技术大学 | The enriching and purifying equipment of pure gas in mixed gas |
| CN110146640A (en) * | 2019-06-03 | 2019-08-20 | 中国科学院地质与地球物理研究所 | The analysis system and method for micro nitrogen isotope |
| CN110531018A (en) * | 2019-09-20 | 2019-12-03 | 通标标准技术服务(上海)有限公司 | A kind of pocket type method direct injected GC-O/MS test macro and its test method |
| CN111965282A (en) * | 2020-08-18 | 2020-11-20 | 中国地质科学院矿产资源研究所 | Ultra-micro sulfur isotope analysis system and analysis method |
| CN113514315A (en) * | 2021-07-09 | 2021-10-19 | 广东海洋大学 | Device and method for removing water during enrichment determination of nitrous oxide stable isotope |
| CN113624901A (en) * | 2021-07-07 | 2021-11-09 | 自然资源部第三海洋研究所 | Total organic carbon analyzer and stable isotope mass spectrometry combined interface device |
| WO2022126796A1 (en) * | 2020-12-17 | 2022-06-23 | 广州禾信仪器股份有限公司 | Multifunctional gas chromatography-mass spectrometry analysis apparatus and method |
| CN114910593A (en) * | 2022-03-14 | 2022-08-16 | 中海油能源发展股份有限公司 | High-temperature molten carbonate enriched carbon dioxide gas purification system and use method thereof |
| CN115561349A (en) * | 2022-09-21 | 2023-01-03 | 中国地质科学院矿产资源研究所 | N-type zeolite 2 Device and method for testing nitrogen and trioxygen isotopes of O gas and cracked gas of O gas |
| CN117269383A (en) * | 2023-09-05 | 2023-12-22 | 中国科学院深海科学与工程研究所 | Multi-type low Wen Duobu sweeping and concentrating device and sweeping and concentrating method thereof |
-
2017
- 2017-02-20 CN CN201710089645.0A patent/CN106706831A/en active Pending
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107328846A (en) * | 2017-08-10 | 2017-11-07 | 中国科学院长春应用化学研究所 | Mass spectrum sampling system and cooling device |
| CN107941891A (en) * | 2017-10-12 | 2018-04-20 | 中国石油天然气股份有限公司 | A kind of method of C-O isotopes in on-line period measure microcell carbonate |
| CN110095575A (en) * | 2019-05-08 | 2019-08-06 | 中国科学技术大学 | The enriching and purifying equipment of pure gas in mixed gas |
| CN110146640A (en) * | 2019-06-03 | 2019-08-20 | 中国科学院地质与地球物理研究所 | The analysis system and method for micro nitrogen isotope |
| CN110146640B (en) * | 2019-06-03 | 2020-03-24 | 中国科学院地质与地球物理研究所 | System and method for analyzing trace nitrogen isotopes |
| CN110531018A (en) * | 2019-09-20 | 2019-12-03 | 通标标准技术服务(上海)有限公司 | A kind of pocket type method direct injected GC-O/MS test macro and its test method |
| CN111965282A (en) * | 2020-08-18 | 2020-11-20 | 中国地质科学院矿产资源研究所 | Ultra-micro sulfur isotope analysis system and analysis method |
| CN111965282B (en) * | 2020-08-18 | 2023-08-29 | 中国地质科学院矿产资源研究所 | Ultra-trace sulfur isotope analysis system and analysis method |
| WO2022126796A1 (en) * | 2020-12-17 | 2022-06-23 | 广州禾信仪器股份有限公司 | Multifunctional gas chromatography-mass spectrometry analysis apparatus and method |
| CN113624901A (en) * | 2021-07-07 | 2021-11-09 | 自然资源部第三海洋研究所 | Total organic carbon analyzer and stable isotope mass spectrometry combined interface device |
| CN113514315A (en) * | 2021-07-09 | 2021-10-19 | 广东海洋大学 | Device and method for removing water during enrichment determination of nitrous oxide stable isotope |
| CN113514315B (en) * | 2021-07-09 | 2024-01-05 | 广东海洋大学 | Device and method for removing water during enrichment determination of nitrous oxide stable isotope |
| CN114910593A (en) * | 2022-03-14 | 2022-08-16 | 中海油能源发展股份有限公司 | High-temperature molten carbonate enriched carbon dioxide gas purification system and use method thereof |
| CN115561349A (en) * | 2022-09-21 | 2023-01-03 | 中国地质科学院矿产资源研究所 | N-type zeolite 2 Device and method for testing nitrogen and trioxygen isotopes of O gas and cracked gas of O gas |
| CN115561349B (en) * | 2022-09-21 | 2023-08-18 | 中国地质科学院矿产资源研究所 | N (N) 2 Device and method for testing nitrogen and trioxyisotope of O gas and pyrolysis gas thereof |
| CN117269383A (en) * | 2023-09-05 | 2023-12-22 | 中国科学院深海科学与工程研究所 | Multi-type low Wen Duobu sweeping and concentrating device and sweeping and concentrating method thereof |
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Application publication date: 20170524 |
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