CN104101668B - The pin type sample introduction cap of fluid injection opening - Google Patents

The pin type sample introduction cap of fluid injection opening Download PDF

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Publication number
CN104101668B
CN104101668B CN201410272725.6A CN201410272725A CN104101668B CN 104101668 B CN104101668 B CN 104101668B CN 201410272725 A CN201410272725 A CN 201410272725A CN 104101668 B CN104101668 B CN 104101668B
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China
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cap
core
pressure cap
interior pressure
injection port
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CN201410272725.6A
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CN104101668A (en
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孙维贞
余海棠
王肖波
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Northwest Institute of Eco Environment and Resources of CAS
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Cold and Arid Regions Environmental and Engineering Research Institute of CAS
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Abstract

The present invention discloses the pin type sample introduction cap that a kind of liquid note sample mouth uses, it is characterized in that outer pressure cap there is outer pressure cap injection port, interior pressure cap injection port is arranged at interior pressure cap top, pressure cap is had to purge air drain in cap, inner side has two interior pressure caps to purge pore, outer pressure cap and interior pressure cap close fit, bottom margin welding after assembling; Cap core top has cap core bore, the screw thread close fit of screw thread and interior pressure cap inside on cap core, centre has sealing gasket to be tightly connected, and under cap core, screw thread is fixedly connected with the interface spiral of elemental analyser, cap core has carrier gas pipe (mouth) and cap core purge tracheae and purge gas port; Outer pressure cap injection port and interior pressure cap injection port and cap core bore are concentric; Structure fabrication of the present invention is exquisite, and it is convenient to change, and can effectively improve as the accuracy of important system accessory for test number, to solve in fluid sample sample introduction process air to the impact of analysis result.Have good value for applications.

Description

The pin type sample introduction cap of fluid injection opening
Technical field
The present invention relates to all special sample introduction caps being applied to fluid injection opening needle injector sample introduction.
Background technology
In fluid sample carbon, nitrogen, stable hydrogen and oxygen isotopes research instruction moisture source, explore Groundwater movement develop and life system nitrogen cycle etc. in significant, be widely used in the fields such as geoscience, environmental science, life science. especially will play a significant role in the research in the direction such as carbon nitrogen cycle of Global climate change, water resources assessment and management, the ecosystem.
Elemental analyser and the coupling of gas isotope mass spectrometer obtain general application in environmental ecology research field in recent years.Wherein TCEA Pintsch process elemental analyser can realize water Oxygen and Hydrogen isotope ratio test in water sample; N-analyzer can realize measuring containing the isotope analysis of nitrogen element in nitrate nitrogen, nitrite nitrogen, ammonium nitrogen sample in liquid.But find in test process, because injection port exposes in atmospheric environment, needle injector, in the moment from instrument injection port injected sample, can enter in elemental analyser because of nitrogen, nitrogen monoxide, nitrous oxide, carbon dioxide etc. in Atmospheric components the test analysis effect affecting oxygen, nitrogen isotope.
Summary of the invention
In view of above-mentioned, object of the present invention aims to provide a kind of pin type sample introduction cap of fluid injection opening.It is directly installed on the liquid injection interface of elemental analyser, effectively on the impact of mass spectrophotometry, can complete the mensuration of hydrogen, oxygen, nitrogen Stable isotope ratio by deaeration.
The object of the present invention is achieved like this:
A pin type sample introduction cap for fluid injection opening, mainly comprises outer pressure cap, outer pressure cap injection port, interior pressure cap, interior pressure cap purges air drain, interior pressure cap purges screw thread, cap core carrier gas pipe (mouth) under screw thread, cap core on pore, interior pressure cap injection port, cap core, cap core, cap core purges tracheae, cap core purges gas port, cap core bore and elemental analyser.Outer pressure cap has outer pressure cap injection port, interior pressure cap injection port is arranged at interior pressure cap top, has interior pressure cap to purge air drain in interior pressure cap cap, and inner side has interior pressure cap to purge pore, outer pressure cap and interior pressure cap close fit, bottom margin welding after assembling; Cap core top has cap core bore, sealing gasket is had between interior pressure cap and cap core bore, on cap core, screw thread is threaded with interior pressure cap, under cap core, screw thread is connected with the interface thread of elemental analyser (EA), cap core has carrier gas pipe (mouth) and cap core purge tracheae, cap core purges tracheae top purging gas port; Outer pressure cap injection port and interior pressure cap injection port and cap core bore are concentric, and carrier gas pipe is connected with concentric hole.
Advantage of the present invention is:
1, the outer pressure cap of the present invention and interior pressure cap close fit, bottom margin welding after assembling, cap core top has cap core bore, sealing gasket is had between interior pressure cap and cap core bore, on cap core, screw thread revolves with interior pressure cap screw thread and is connected, under cap core, the interface thread of screw thread and elemental analyser (EA) revolves connection, and it is overall that pin type sample introduction cap forms sealing.Fluid sample enters into elemental analyser by pin type sample introduction cap injection port and cap core bore, effectively can stop the impact of air, fluid sample is made to guarantee the pure of sample introduction environment in injection transient by sweep gas, pollute impact on instrument test background after avoiding composition of air to enter elemental analyser, increase the stability of sample analysis.Structure fabrication of the present invention is exquisite, and it is convenient to change, and can effectively improve as the accuracy of important system accessory for test number, and cost of manufacture is low simultaneously, long service life.
2, the present invention can be applicable to the fluid injection opening of any device, reduce Sample Injection link air to the impact of nitrogen, oxygen element composition dependence test result, stability and the measuring accuracy of test analysis are all greatly improved, and have good value for applications.
Accompanying drawing explanation
Fig. 1 is pin type sample introduction cap schematic diagram.
Fig. 2 is Fig. 1 China and foreign countries cap figure.
Fig. 3 is interior cap figure in Fig. 1.
Fig. 4 is Fig. 1 China and foreign countries' cap and interior cap cooperation figure.
Fig. 5 is cap core schematic diagram in Fig. 1.
Embodiment
Below, by reference to the accompanying drawings, technical scheme of the present invention is further described again:
As Figure 1-5, a kind of pin type sample introduction cap of fluid injection opening, be mounted on elemental analyser liquid injection port part, for the front device of hydrogen, oxygen, nitrogen isotope test in analyzing liquid sample, mainly comprise outer pressure cap 1, outer pressure cap injection port 2, interior pressure cap 3, interior pressure cap purges air drain 4, interior pressure cap purges screw thread 9, cap core carrier gas pipe (mouth) 10 under screw thread 8, cap core on pore 5, interior pressure cap injection port 6, cap core 7, cap core, cap core purges tracheae 11, cap core purges gas port 12, cap core bore 13 and elemental analyser 14.Outer pressure cap 1 there is outer pressure cap injection port 2, interior pressure cap injection port 6 is arranged at interior pressure cap 3 top, has interior pressure cap to purge air drain 4 in interior pressure cap cap, and inner side has two interior pressure caps to purge pore 5, outer pressure cap 1 and interior pressure cap 3 close fit, outer pressure cap 1 and the welding of interior pressure cap 3 bottom margin after assembling; Cap core 7 top has cap core bore 13, sealing gasket is had between interior pressure cap 3 and cap core bore 13, on cap core, screw thread 8 is threaded with interior pressure cap 3, under cap core, screw thread 9 is connected with the interface thread of elemental analyser (EA) 14, cap core 7 has carrier gas pipe (mouth) 10 and cap core purge tracheae 11, cap core purges tracheae 11 top purging gas port 12; Outer pressure cap injection port 2 and interior pressure cap injection port 6 and cap core bore 13 are concentric, and carrier gas pipe 10 is connected with concentric hole.
Carrier gas by cap core carrier gas pipe (mouth) 10 by carry in concentric hole from pin type sample introduction cap inject fluid sample, reacted gas componant in elemental analyser (EA) 14 is sent in isotope mass spectrometer (MS) 16 after chromatographic column (GC) 15 is separated, completes the analytical test to nitrogen, stable hydrogen and oxygen isotopes in fluid sample.
Specific implementation process follows these steps to carry out (Hydrogen-oxygen Isotope in test water)
I) hunt leak: before sample test, first want adjustment cap core carrier gas pipe 10 and cap core to purge the flow of tracheae 11 place two-way helium; GC/PAL liquid automatic sampler (if do not have automatic sampler, use hand sampling mode) set the three dimensional space coordinate of syringe and pin type sample introduction cap; Then to the interface of screw thread 9 under the cap core carrier gas mouth of pipe 10 of pin type sample introduction cap, outer pressure cap injection port 2, cap core and elemental analyser 14, chromatographic column (GC) 15 interface and be connected isotope mass spectrometer (MS) 16 the junction such as needle-valve respectively with the leak detection of Ar gas, guarantee that each link of system connects without leak source.
II) purge sample introduction: the intensification leak detection program starting elemental analyser, get rid of and temperature (1400 at gas leakage point oc) stable rear drive GC/PAL liquid automatic sampler, fluid sample is injected by the outer pressure cap injection port 2 of pin type sample introduction cap after automatic sampler sampling, before fluid sample injects sample introduction cap, start sweep gas and purge program (in computer testing program, can purge time be set), at this moment sweep gas (helium) by purge gas port 12 enter interior pressure cap purge air drain 4 connected ring around after purge pore 5 from interior pressure cap and continue blowout, avoid composition of air as CO 2,n 2,nO, N 2o etc. enter pollutant's spectrometer 16, maintain the cleaning in pin type sample introduction cap sample introduction space.Then, fluid sample is injected cap core bore 13, together enter in the reaction tube of elemental analyser 14, in elemental analyser (EA) 14, reacted gas componant is sent in isotope mass spectrometer (MS) 16 after chromatographic column (GC) 15 is separated, and completes the analytical test to stable hydrogen and oxygen isotopes in fluid sample.
III) analytical test: fluid sample enters in elemental analyser 14 with the carrier gas of cap core carrier gas pipe (mouth) 10 and following chemical reaction occurs: H 2o+C → H 2+ CO, reacted H 2enter after chromatographic column (GC) 15 with CO gas and be separated, the H after separation 2successively send in mass spectrometer 16 respectively by kapillary with CO, complete the mensuration of stable hydrogen and oxygen isotopes ratio; Shut-down purge gas after Sample Injection, can save sweep gas like this, reduces testing cost.
Similarly, in the fluid sample of test containing salts such as ammonium nitrogen, nitrate nitrogen, nitrite nitrogens during nitrogen isotope, there is following oxidation, reduction reaction respectively:
Ammonium nitrogen: 2NH 4 ++ 3BrO -+ 2OH -→ N 2+ 3H 2o+3Br -
Nitrate nitrogen: NO 2 -+ 2KI+H +→ NO+KII+KOH
Nitrite nitrogen: NO 3 -+ V 3++ 4H +→ NO+3V 4++ 2H 2o
Can find out, after the above-mentioned salt sample containing various valence state nitrogen carries out chemical reaction in elemental analyser, generate N2 or NO, air (N2, NO, N in space 2o) existence of composition, is bound to impact test result.Design and use of the present invention, eliminate the composition of air at injection port place, keep the cleaning of sample introduction time space under the maintenance of sweep gas, decrease CO in air 2,n 2,nO, N 2o composition, on the impact of oxygen and nitrogen isotope value in the impact of instrument test background and test, improves the precision and stability of sample test.

Claims (1)

1. a pin type sample introduction cap liquid note sample mouth used, mainly comprise outer pressure cap (1), outer pressure cap injection port (2), interior pressure cap (3), interior pressure cap purges air drain (4), interior pressure cap purges pore (5), interior pressure cap injection port (6), cap core (7), screw thread (8) on cap core, screw thread (9) under cap core, cap core carrier gas pipe (10), cap core purges tracheae (11), cap core purges gas port (12), cap core bore (13), described pin type sample introduction cap is directly installed on the liquid note sample mouth of elemental analyser (14), it is characterized in that outer pressure cap (1) there is outer pressure cap injection port (2), interior pressure cap injection port (6) is arranged at interior pressure cap (3) top, interior pressure cap is had to purge air drain (4) in interior pressure cap cap, inner side has interior pressure cap to purge pore (5), outer pressure cap (1) and interior pressure cap (3) close fit, bottom margin welding after assembling, cap core (7) top has cap core bore (13), sealing gasket is had to seal between interior pressure cap (3) and cap core bore (13), on cap core, screw thread (8) is threaded with interior pressure cap (3), under cap core, screw thread (9) is connected with the interface thread of elemental analyser (14), cap core (7) has cap core carrier gas pipe (10) and cap core purge tracheae (11), cap core purges tracheae (11) top purging gas port (12), outer pressure cap injection port (2) and interior pressure cap injection port (6) and cap core bore (13) are concentric, and cap core carrier gas pipe (10) is connected with concentric hole.
CN201410272725.6A 2014-06-18 2014-06-18 The pin type sample introduction cap of fluid injection opening Active CN104101668B (en)

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US6035697A (en) * 1996-11-11 2000-03-14 Sgt Exploitatie B.V. Gas chromatograph apparatus
CN2738252Y (en) * 2004-11-04 2005-11-02 上海科创色谱仪器有限公司 Capillary column and filling column two purpose sampler for gas chromatography
CN2826428Y (en) * 2005-02-04 2006-10-11 安捷伦科技有限公司 Gas chromatograph injection port with improved sealing device
CN102636659A (en) * 2012-05-09 2012-08-15 长沙瑞翔科技有限公司 Automatic sampling device
CN203432985U (en) * 2013-01-23 2014-02-12 中国科学院寒区旱区环境与工程研究所 Solid sampling disc directly applied to automatic sampler of elemental analyzer

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Effective date of registration: 20200818

Address after: 730000 No.318, Donggang West Road, Chengguan District, Lanzhou City, Gansu Province

Patentee after: NORTHWEST INSTITUTE OF ECO-ENVIRONMENT AND RESOURCES, CAS

Address before: Chengguan District of Gansu city of Lanzhou province Donggang West Road 730000 No. 320

Patentee before: Institute of environment and Engineering in cold and dry areas, Chinese Academy of Sciences