CN108107145A - Gas concentration instrument - Google Patents
Gas concentration instrument Download PDFInfo
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- CN108107145A CN108107145A CN201711316727.0A CN201711316727A CN108107145A CN 108107145 A CN108107145 A CN 108107145A CN 201711316727 A CN201711316727 A CN 201711316727A CN 108107145 A CN108107145 A CN 108107145A
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- way valve
- tube body
- pipe
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- 239000007789 gas Substances 0.000 claims abstract description 105
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 77
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 39
- 238000005070 sampling Methods 0.000 claims abstract description 33
- 239000001307 helium Substances 0.000 claims abstract description 15
- 229910052734 helium Inorganic materials 0.000 claims abstract description 15
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000007710 freezing Methods 0.000 claims description 24
- 230000008014 freezing Effects 0.000 claims description 24
- 239000007788 liquid Substances 0.000 claims description 21
- 238000009413 insulation Methods 0.000 claims description 14
- 238000003860 storage Methods 0.000 claims description 12
- 238000010276 construction Methods 0.000 claims description 5
- 238000005452 bending Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 238000002444 silanisation Methods 0.000 claims description 3
- 230000005532 trapping Effects 0.000 claims description 3
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical compound FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims description 2
- 239000005416 organic matter Substances 0.000 abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 6
- 238000004458 analytical method Methods 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 14
- 238000010926 purge Methods 0.000 description 9
- 239000012855 volatile organic compound Substances 0.000 description 9
- 229910002092 carbon dioxide Inorganic materials 0.000 description 7
- 239000001569 carbon dioxide Substances 0.000 description 7
- 238000012544 monitoring process Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 238000000746 purification Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 238000001816 cooling Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 150000002894 organic compounds Chemical class 0.000 description 4
- 230000001133 acceleration Effects 0.000 description 3
- 238000004587 chromatography analysis Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 239000000571 coke Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 238000003032 molecular docking Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000005057 refrigeration Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000008719 thickening Effects 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 125000002619 bicyclic group Chemical group 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000004868 gas analysis Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000003694 hair properties Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/16—Injection
- G01N30/20—Injection using a sampling valve
-
- 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
-
- 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
- G01N30/16—Injection
- G01N30/20—Injection using a sampling valve
- G01N2030/201—Injection using a sampling valve multiport valves, i.e. having more than two ports
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The present invention provides gas concentration instrument, the front end of gas chromatograph is placed in, including sampling device, ten-way valve, six-way valve, capturing device, discharger, helium input pipe, cold focusing arrangement；The capturing device is quantity tube；The sampling device further includes ten-way valve, autosampler and six sample input pipes, internal standard input pipe and nitrogen input pipe.Gas concentration instrument provided by the present invention is a instrument for being directly connected to gas chromatograph and doing high concentration chemical analysis, and the volatile organic matter of high quality is provided for gas chromatograph.It is with sampling device, it can realize while there are 22 road sample intake passages, and wherein 16 paths realize automatic sampling, the Soviet Union's agate tank or airbag of complete series size can be connect, it is with cold focusing arrangement, the temperature of its cold focusing can be controlled at 100 DEG C to 196 DEG C, can realize that sample focuses on again under cryogenic so that sample is being less than 1 microlitre into the volume before gas chromatograph.
Description
Technical field
The present invention relates to gas detection equipment technical field, more particularly, to a kind of gas concentration instrument.
Background technology
In environmental monitoring and analysis technical field, the volatile organic matter in air or exhaust gas is Evaluation Environment quality
Important indicator, volatile organic matter is monitored and analyzed be environmental monitoring emphasis, it is significant.It is existing to be directed to volatility
There are cryotraps using electronic cooling technology for the device for monitoring and analyzing of organic matter, be unable to reach deep cooling (- 195 DEG C) and nothing
Method traps low-boiling volatile organic matter, and the adsorbent in trap tube quantifies, and absorption is easily saturated and needs several samples
The monitoring effect of gas concentration instrument is poor caused by the problems such as carrying out needing manual operation sample introduction during sample introduction, manual operation error
Greatly, data deviate authenticity, the result error of data is big, linear and reappearance is inconsistent.
The content of the invention
Poor it is an object of the invention to solve the monitoring effect of existing gas concentration instrument, manual operation error is big, data are inclined
The shortcomings that result error from authenticity, data is big, linear and reappearance is inconsistent, provides a kind of gas concentration instrument.
The present invention solve its technical problem the technical solution adopted is that：Gas concentration instrument is placed in the front end of gas chromatograph,
Including sampling device, six-way valve, capturing device, discharger, helium input pipe, cold focusing arrangement；
The sampling device includes sample feeding pipe；
The capturing device is quantity tube, and the quantity tube is 1/16 inch of silanization pipe, has first port and the
Two-port netwerk；
The discharger include four-way valve, be connected with the 18th interface of the four-way valve emptying discharge line, and
The efferent duct with vacuum pump of the 19th interface connection of the four-way valve；
The cold focusing arrangement has the housing of freezing chamber, is equipped with sample input in the housing and sample exports
End, the sample output terminal are connected with the gas chromatograph；
11st interface of the six-way valve is connected with the sample feeding pipe of the sampling device, the 12nd interface and the discharge
The 17th interface connection of the four-way valve of device, the of the 13rd interface of the six-way valve and the quantity tube of the capturing device
Single port connects, and the 16th interface of the six-way valve is connected with the second port of the quantity tube of the capturing device, and described six
14th interface of port valve is connected with the helium input pipe, the sample of cold focusing arrangement described in the 15th interface of the six-way valve
Product input terminal connects.
Further, the sampling device further includes ten-way valve, autosampler and six sample input pipes；Described ten
The first interface of port valve is connected with the input pipe of the autosampler, and second interface, the 3rd interface, the 4th interface, the 8th connect
Mouth, the 9th interface and the tenth interface are connected respectively with six sample input pipes, and the 7th interface is connected with the sample feeding pipe.
Further, the cold focusing arrangement further includes the liquid nitrogen being placed in outside the housing, is provided on the housing
Outlet for the input port for inputting liquid nitrogen and for discharging liquid nitrogen is provided with to convey the of sample in the freezing chamber
One tube body and the second tube body for being heated after freezing to first tube body, first tube body are threaded through institute
It states in the second tube body and bending is provided with deformation structure, be provided with insulation construction at the deformation structure, described first
One end of tube body is connected with the sample input, and the other end is connected with the sample output terminal, the both ends of second tube body
Head first tube body between be respectively formed be useful for input heat gas air inlet and for for heat gas discharge
Exhaust outlet.
Further, the cold focusing arrangement further includes gas blow pipe, the air inlet of the gas blow pipe and second tube body
Connection.
Specifically, first tube body is metal tube, and the second tube body is 1/8 inch of tetrafluoroethene pipe.
Specifically, the caliber of first tube body is less than the caliber of second tube body.
Further, the discharger further includes mass flowmenter, and the mass flowmenter is placed in the four-way valve
Between 19th interface and the vacuum pump.
Specifically, the autosampler includes free switching device and provides depositing for sample for the free switching device
Storage device, the free switching device include 16 port valves and dock the inlet channel in 16 port valve with output channel
Switching device, the output channel are connected with the first interface of the ten-way valve.
Specifically, the sampling device further includes internal standard input pipe, and the 5th interface of the ten-way valve and the internal standard are defeated
Enter pipe connection.
Specifically, the sampling device further includes nitrogen input pipe, and the 6th interface of the ten-way valve and the nitrogen are defeated
Enter pipe connection.
The beneficial effects of the present invention are：Gas concentration instrument provided by the present invention is a to be directly connected to gas phase color
Spectrometer makees the instrument of high concentration chemical analysis, and the volatile organic matter of high quality is provided for gas chromatograph, is widely used in
The fields such as oil, chemistry, agriculture chemistry, biochemistry, medical and health, food.Gas concentration instrument provided by the present invention, tool
There is sampling device, can realize while there are 22 road sample intake passages, and wherein 16 paths realize automatic sampling, can connect complete set
The Soviet Union's agate tank or airbag of row size, with cold focusing arrangement, the temperature of cold focusing can be controlled at -100 DEG C to -196 DEG C,
It can realize that sample focuses on again under cryogenic so that sample is being less than 1 microlitre into the volume before gas chromatograph.
Description of the drawings
Fig. 1 is the conduit line map of gas concentration instrument provided in an embodiment of the present invention；
Fig. 2 is the dimensional structure diagram of gas concentration instrument provided in an embodiment of the present invention；
Fig. 3 is the structure diagram of the cold focusing arrangement of gas concentration instrument provided in an embodiment of the present invention；
Fig. 4 is the broken section of the free switching device of the autosampler of gas concentration instrument provided in an embodiment of the present invention
Figure；
In figure：100- gas concentration instrument
10- sampling device 11- sample feeding pipe 12- ten-way valves
The second interface of the first interface P2- ten-way valves of P1- ten-way valves
4th interface of the 3rd interface P4- ten-way valves of P3- ten-way valves
6th interface of the 5th interface P6- ten-way valves of P5- ten-way valves
8th interface of the 7th interface P2- ten-way valves of P7- ten-way valves
Tenth interface of the 9th interface P10- ten-way valves of P9- ten-way valves
13- sample input pipe 14- internal standard input pipe 15- nitrogen input pipes
20- capturing device 21- quantity tube 22- first port 23- second ports
30- discharger 31- four-way valves 32- is vented discharge pipe
33- efferent duct 34- vacuum pump 35- mass flowmenters
18th interface of the 17th interface S2- four-way valves of S1- four-way valves
20th interface of the 19th interface S4- four-way valves of S3- four-way valves
The cold focusing arrangement 41- housings 411- freezing chambers of 40-
412- main body 413- head cover 42- sample input 43- sample output terminals
44- liquid nitrogen 441- input ports 442- delivery outlets
45- the first tube body 46- the second tube body 461- air inlet 462- gas outlets
47- deformation structure 48- gas blow pipe 493- temperature detectors
49- insulation construction 491- thermal insulation board 492- insulation covers
50- six-way valve 60- helium input pipe 70- gas chromatographs
12nd interface of the 11st interface G2- six-way valves of G1- six-way valves
14th interface of the 13rd interface G4- six-way valves of G3- six-way valves
16th interface of the 15th interface G6- six-way valves of G5- six-way valves
80- autosampler 81- switching device 83-16 port valves
82- storage device 821- storage rack 822- gas storage device 823- stainless steel tubes
831- toroidal shell 832- circle spool 833- inlet channel 834- output channels
84- stepper motor 85- driver 86- index dial 87- photoelectrical couplers
89- mainboards
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, it is right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
It is gas concentration instrument 100 provided by the present invention referring to Fig. 1-2, the front end of gas chromatograph is placed in, including sample introduction
Device 10, six-way valve 50, capturing device 20, discharger 30, helium input pipe 60, cold focusing arrangement 40.It is provided by the present invention
Gas concentration instrument 100, be a instrument for being directly connected to gas chromatograph 70 and doing high concentration chemical analysis.It is with sample introduction
Device 10 is equipped with autosampler 80 in sampling device 10, can realize and automatically switch sample introduction access, can disposably set
The sample introduction operation of 16 kinds of different samples is put, therefore plus original six sample intake passages so that gas provided by the present invention is dense
Contracting instrument 100 can have 22 road sample intake passages simultaneously, can connect the Soviet Union's agate tank or airbag of complete series size.And gas concentration instrument
100 also have cold focusing arrangement 40, and the temperature of cold focusing can be controlled at -100 DEG C to -196 DEG C, and sample can be realized in depth
It is focused on again under cold state so that sample is being less than 1 microlitre into the volume before gas chromatograph.
Specifically, referring again to Fig. 1-2, sampling device 10 provided by the present invention includes sample feeding pipe 11；It is logical to further include ten
Valve 12, autosampler 80 and six sample input pipes 13；The wherein first interface P1 of ten-way valve 12 and autosampler 80
Input pipe connects, second interface, the 3rd interfaces of P2, the 4th interface P4 of P3, the 8th interface, the 9th interface P9 of P8 and the tenth interface
P10 is connected respectively with six sample input pipes 13, and the 7th interface P7 is connected with sample feeding pipe 11.
The sampling device 10 not only has 6 sample input pipes 14, also with internal standard input pipe 14, the 5th of ten-way valve 12 the
Interface P5 is connected with internal standard input pipe 14.Internal standard is added in sampling device 10, effect is the system change to gas concentration instrument 100
It is turned into compensation monitoring, adds in internal standard and can obviously reduce error, without correcting data.
Meanwhile the sampling device 10 further includes nitrogen input pipe 15, the 6th interface P6 and the nitrogen input pipe of ten-way valve 12
15 connections.The nitrogen input pipe 15 can complete the purging cleaning system of all pipelines in gas concentration instrument 100, in pipeline
Sample carryover purged.
Further, the sampling device 10 of gas concentration instrument 100 provided by the present invention also has autosampler 80, should
Autosampler 80 can access 16 sample paths simultaneously, and then its 16 sample paths are carried out by automatic switching control equipment 81
Selection, select need sample path connected with output channel 834, so as to can output channel 834 output sample finally from
The first interface P1 of ten-way valve 12 enters in sample feeding pipe 11.
Then, referring to attached drawing 2 and Fig. 4, for the structure chart of autosampler 80 provided by the present invention.The autosampler
80 include free switching device 81 and the storage device 82 of sample are provided for free switching device 81, and free switching device 81 includes
16 port valves 83 and the switching device for docking the inlet channel 833 in 16 port valves 83 with output channel 834, output channel 834
It is connected with the first interface P1 of ten-way valve 12.16 port valves 83 in the autosampler 80 include a toroidal shell 831 and position
In the circular spool 832 that can be rotated in toroidal shell 831 compared with toroidal shell 831.Toroidal shell 831 is equipped with 16 air inlets
Passage 833 and 1 output channel 834, set that there are one the inputs rotatably, with inlet channel 833 connected on circular spool 832
Port (not showing place in figure) and an output port connected with output channel 834.16 port valve 83 is by circular spool
832 in toroidal shell 831 relative rotation, so as to by the input port on the circle spool 832 and toroidal shell 831 into
Gas passage 833 docks, so as to which sample can be by inlet channel 833 into circular spool 832, then from circular spool 832
Output channel 834 is connected at output port, is exported at output channel 834.And it is selected not by the rotation of circular spool 832
Same inlet channel 833 realizes the selection of the sample introduction access of autosampler 80.The autosampler 80 passes through switching device 81
Realize the input port of circular spool 832 and the docking for inlet channel 833 automatically controlled in 16 port valves 83.The switching device 81
Including being fixedly connected with the stepper motor 84 that it can be driven to rotate with the circular spool 832 of 16 port valves 83, powering for stepper motor 84
Driver 85 and control the mainboard 89 of driver 85, mainboard 89 is electrically connected with gas concentration instrument 100.The switching device 81
Mainboard 89 be subject to the control of gas concentration instrument 100, gas concentration instrument 100 sends autosampler 80 demand, and mainboard 89 is controlled
Driver 85 processed is powered for stepper motor 84, and stepper motor 84 drives circular spool 832 to rotate, when the input of circular spool 832
Port is rotated at inlet channel 833, which connects with circular spool 832, and sample enters circular spool 832, so
It is exported afterwards from output channel 834.Stepper motor 84 provided by the present invention is a kind of induction machine, its operation principle is to utilize
Direct current is become time sharing power supply by electronic circuit, and multiphase timing control electric current is that stepper motor 84 is powered with this electric current,
Stepper motor 84 could work normally.Driver 85 is exactly for stepper motor time sharing power supply, multiphase time schedule controller.Driver 85
It must can be used by forming control systems such as bicyclic shaped pulse signal, power driving circuits.When driver 85 is subject to mainboard 89
Pulse signal, it with regard to Driving Stepping Motor by setting direction rotate a fixed angle, by control pulse number come
Angular displacement is controlled, pulse frequency can also be controlled to control the speed and acceleration of motor rotation, so as to reach the mesh of speed governing
's.I.e. switching device 81 can control the rotary speed of stepper motor 84 and the rotation angle of acceleration and stepper motor 84,
That is the switching device 81 is controlled the angle of the rotation of the circular spool 832 in 16 port valves 83 by stepper motor 84, is somebody's turn to do
The rotary speed and acceleration of circular spool 832.The switching device 81 further includes point being fixedly and coaxially connected with circular spool 832
Scale 86 and be electrically connected with driver 85 for detecting the photoelectrical coupler 87 of 86 rotation angle of index dial, set on index dial 86
There are 16 circumferentially equally distributed through holes.On index dial 86 circumferentially on be uniformly distributed 16 through holes, the through hole and 16 logical
16 inlet channels 833 on valve 83 are one-to-one.The switching device 81 is true by index dial 86 and photoelectrical coupler 87
The rotation angle of fixed circle spool 832 when stepper motor 84 drives circular spool 832 to rotate, while drives and circular spool
832 co-axially fixed index dials 86 rotate, when rotating to the through hole on index dial 86, the light of 87 transmitting terminal of photoelectrical coupler
When penetrating the through hole of index dial 86, photoelectrical coupler 87, which receives signal and feeds back to driver 85, to stop operating, accurate so as to reach
Determine the effect of 16 inlet channels 833 in 16 port valve 83 of position.The storage device 82 of autosampler 80 provided by the present invention
16 gas storage devices 822 including storage rack 821 and in storage rack 821,822 and 16 port valve of gas storage device
83 inlet channel 833 is connected by stainless steel tube 823.The gas storage device 823 is Soviet Union's agate tank or airbag.Gas stores
Device 823 can be complete series size (1L 3L 6L 15L) Soviet Union's agate tank or airbag.Soviet Union's agate tank or airbag pass through stainless steel
Pipe 823 accesses the inlet channel 833 of 16 port valves 83.
Further, gas concentration instrument 100 provided herein includes capturing device 20, which is quantitative
Pipe 21, quantity tube 21 are 1/16 inch of silanization pipe, have first port 22 and second port 23.Sample is carried out by quantity tube 21
Product it is quantitative (the volume size of replaceable quantity tube 21,0.2L 0.5 1L 2L).The quantity tube 21 is waved the whole in sample
The captures such as hair property organic compound, water and carbon dioxide.Quantity tube 21 parses volatile organic compounds to cold focusing with room temperature
Device 40 has different vapour pressures using volatile organic compounds and moisture content during shifting, and moisture content is stayed in quantity tube
In 21, afterwards quantity tube 21 on sampling device 10 nitrogen input pipe 15 input nitrogen carry out purging purification will be in quantity tube 21
Sample carryover purges.
Further, gas concentration instrument 100 provided herein, which includes discharger 30, includes four-way valve 31 and four-way
The emptying discharge line 32 of 18th interface S2 connections of valve 31, be connected with the 19th interface S3 of four-way valve 31 have vacuum
The efferent duct 33 of pump 34；The discharger 30 further includes mass flowmenter 35, and mass flowmenter 35 is placed in the tenth of four-way valve 31
Between nine interface S3 and vacuum pump 34.The discharger 30 has two discharge lines, and an emptying discharge line 32 is used for will
Exhaust gas in sample etc. is discharged without the sample of monitoring from emptying discharge line 32, another efferent duct with vacuum pump 34
33 detect whether volatile organic compounds, water and carbon dioxide in quantity tube 21 etc. has captured by mass flowmenter 35
Entirely, when mass flowmenter 35 reaches setting flow, sample introduction is closed, and the sample of trapping in quantity tube 21 be transferred to cold poly-
Cold focusing is carried out in coke installation 40.
Further, referring to attached drawing 1 and attached drawing 3, cold focusing arrangement is included for gas concentration instrument 100 provided herein
40 have the housing 41 of freezing chamber 411, and sample input 42 and sample output terminal 43, sample output terminal 42 are equipped in housing 41
It is connected with gas chromatograph 70.Cold focusing arrangement 40 is provided in gas concentration instrument 100 provided by the present invention, which fills
Quantity tube 21 can be shifted the sample refocusing to come by putting 40 so that sample is less than into the volume before gas chromatograph 70
1 microlitre.Cold focusing arrangement 40 is using the cold type of focusing before chromatographic column, makes the volatilization after thickening, carbon dioxide removal
Property organic compound further concentration focus on capillary chromatography column cap, be then rapidly heated make it into chromatographic column complete chromatography
Analysis.The cold focusing arrangement 40 is interior from quantity tube by the first tube body 45 using input liquid nitrogen 44 is first passed through in freezing chamber 411
The sample that 21 transfers come is freezed, then again by inputting heat gas into the second tube body 46 come fast after freezing
Sample in speed the first tube body 45 of heating, such set-up mode make full use of the characteristics of each ingredient properties are different in sample, rear
In continuous 70 analytic process of gas chromatograph, realize the image that can compose different peak shapes, and peak shape it is higher, it is sharp, separated
It is whole, do not trail, figure is good-looking, improves the convenience of gas analysis and the accuracy of data.
Specifically, the cold focusing arrangement 40 in gas concentration instrument 100 provided by the present invention, which further includes, is placed in outside housing 41
Liquid nitrogen 44, in the input port 441 for being provided with to input liquid nitrogen 44 on housing 41 and outlet for discharging liquid nitrogen 44
442, be provided in freezing chamber 411 to convey the first tube body 45 of sample and for after freezing to the first tube body 45 into
Second tube body 46 of row heating, the first tube body 45 is threaded through in the second tube body 46 and bending is provided with deformation structure 47, is located at
Insulation construction 49 is provided at deformation structure 47, one end of the first tube body 45 is connected with sample input 42, the other end and sample
Output terminal 43 connects, be respectively formed between the two ends of the second tube body 46 and the first tube body 45 be useful for input heat gas into
Gas port 461 and the exhaust outlet 462 for being discharged for heat gas.
Further, after cold focusing arrangement 40 completes the sample being transferred out to quantity tube 21 cold focusing, by setting
The gas blow pipe 48 put completes sample presentation.The gas blow pipe 48 is connected with the air inlet 462 of the second tube body 46.It will be cold poly- by gas blow pipe 48
Sample in first tube body 45 of coke installation 40, which is transferred in gas chromatograph 70, to be analyzed.
Setting in this way, sample to be analyzed utilize liquid nitrogen before the chromatographic column of gas chromatograph 70 is entered
44 effect can freeze the sample in the first tube body 45 in freezing chamber 411.And at the end of freezing, it is heated using outside
Gas is inputted from air inlet 461, and is flowed out from exhaust outlet 462, and heat gas is while stream is by the second tube body 46, the
Sample with volatile organic compounds gas quick heating, and the sample in the first tube body 45 is turned simultaneously in one tube body 45
It moves in chromatographic column, thus on the same time, using the characteristic of volatile organic compounds itself, fireballing organic compound
Object gas just can compose peak shape figure earlier, and the organic compound to pull up lame will compose peak shape figure in glue evening, real at this time
The image of different peak shapes can be composed by having showed, and peak shape is higher, sharp, separation is complete, does not trail, and figure is good-looking.In order to meet
Testing requirement and is set, reduces the body of housing 41 for convenience, it is necessary to the first tube body 45 and the second tube body 46 are set longer
Product, will pass through and be both provided with deformation structure 47 on the first tube body 45 and the second tube body 46, so that the first tube body 45 and second
Tube body 46 not only meets testing requirement in the longitudinal direction, but also can also reduce the volume of housing 41, is easily installed, and reduces manufacture
Cost.And the setting of insulation construction 49, so that when refrigerant is in cryogenic refrigeration sample, the balance of temperature can be kept.The guarantor
Warm structure 49 include thermal insulation board 491 and insulation cover 492, insulation cover 492 lid close on thermal insulation board 491 and between be formed with heat preservation
Chamber, deformation structure 47 are arranged in incubation cavity.So as to which the common insulation for leading to the thermal insulation board 491 and insulation cover 492 acts on, it is ensured that
The balance of temperature can be kept when liquid nitrogen cryogenic refrigeration.As shown in figure 3, during specific manufacture, which includes one end open
Main body 412 and for cover close sealed opening head cover 413, head cover 413 is connected by connection structure with main body 412, and is freezed
Chamber is then formed in main body 412, and the first tube body 45 and the second tube body 46 are pierced by from the bottom of main body 412.
In the present embodiment, during freezing, liquid nitrogen 44 is input in freezing chamber 411 by input port 441, then liquid nitrogen 44
After being expanded in freezing chamber 411, sprayed via delivery outlet 442, in this process, liquid nitrogen can be quickly by freezing chamber
Temperature in 411 is refrigerated to set temperature.The liquid nitrogen is provided by external liquid nitrogen container.And due to temperature height in freezing chamber 411
Low control is controlled by liquid nitrogen flow size, thus in order to realize and the temperature in freezing chamber 411 can be controlled, just
Be provided with to detect the temperature detector 493 of cavity temperature in freezing chamber 411, so as to by the temperature detector 493 come
The temperature in freezing chamber 411 is measured, the temperature then detected via control software collecting temperature detector 493, then realize to system
The control of cryogen uninterrupted.The temperature detector 493 is thermocouple.For the accurate temperature detected in freezing chamber 411
The temperature detector 493, is just located at exhaust outlet 462 by degree.
Preferably, in embodiments of the present invention, deformation structure 47 is in " U-shape ".Gas flowing is not only convenient for, and can be had
Volume occupied by effect the first tube body 45 of reduction and the second tube body 46.As another realization method of deformation structure 47, may be used also
Deformation structure 47 is set in " helical form ", can be end to end circuitous configuration, equally disclosure satisfy that use demand.
Preferably, in specific manufacture, the first tube body 45 is metal tube, and the second tube body 46 is 1/8 inch of tetrafluoro second
Alkene pipe.The caliber of first tube body 45 is less than the caliber of the second tube body 46, so that it is guaranteed that can penetrate into the second tube body 13.
Further, gas concentration instrument 100 provided herein includes the 11st interface G1 and sample introduction of six-way valve 50
The sample feeding pipe 11 of device 10 connects, and the 12nd interface G2 is connected with the 17th interface S1 of the four-way valve 31 of discharger 30, and six
13rd interface G3 of port valve 50 is connected with the first port 22 of the quantity tube 21 of capturing device 20, and the 16th of six-way valve 50 connects
Mouth G6 is connected with the second port 23 of the quantity tube 21 of capturing device 20, the 14th interface G4 and the helium input pipe of six-way valve 50
60 connections, the sample input 42 of the cold focusing arrangements 40 of the 15th interface G5 of six-way valve 50 connect.
In opening, the 11st interface G1 and the 16th interface G6 are connected the six-way valve 50, i.e., sample feeding pipe 11 is with determining
The second port 23 of buret 21 is connected；12nd interface G2 and the 13rd interface G3 is connected, i.e. the four-way valve 31 of discharger 30
The first port 22 of the 17th interface S1 and quantity tube 21 connect；The 15th interface G5 of 14th interface G4 are connected, i.e. helium
Input pipe 60 and the sample input 42 of cold focusing arrangement 40 are connected.
Six-way valve 50 in off position when, the 11st interface G1 and the 12nd interface G2 are connected, i.e. sample feeding pipe 11 and four-way
17th interface S1 of valve 31 is connected；13rd interface G3 and the 14th interface G4 is connected, i.e. the first port 22 of quantity tube 21
It is connected with helium input pipe 60；15th interface G5 and the 16th interface G6 is connected, i.e., the sample input of cold focusing arrangement 40
42 connect with the second port 23 of quantity tube 21.
The operation principle of gas concentration instrument provided by the present invention is：By sampling device, capturing device, discharger,
Cold focusing arrangement, six-way valve control the gas flow path under various working conditions, so as to fulfill the concentration of volatile organic matter, and then
The volatile organic matter of high quality is provided for gas chromatograph.
The course of work of gas concentration instrument provided by the present invention is as follows：
1st, sample purge pipeline：Sample enters from autosampler 80 in 12, all parts in gas concentration instrument 100
When temperature reaches stable, sample from autosampler 80 into gas concentration instrument 100 in, sample according to the flow velocity that sets and when
Between pipeline in purge gas concentrating instrument 100.
2nd, internal standard sample introduction：At this point, six-way valve 50 is in opening, internal standard gas is logical into ten by internal standard input pipe 14
In valve 12, and pass through sample feeding pipe 11 and enter six-way valve 50, then entered by six-way valve 50 in quantity tube 21 and quantified, and it is final
It is exported from the efferent duct 33 with vacuum pump 34 of discharger 30.
3rd, sample feeding：Six-way valve 50 is opened, and sample to be detected can pass through the autosampler in sampling device 10
80 carry out automatic sampling, can also pass through sampling device 10 by the 13 artificial sample introduction of sample introduction input pipe of sampling device 10, sample
The 7th interface P7 of ten-way valve 12 enter in sample feeding pipe 11, sample to be detected at this time passes through sample feeding pipe 11 and enters six-way valve 50
11st interface G1, sample is directly input into the 16th interface G6 in six-way valve 50), i.e., sample is entered by the 16th interface G6
The second port 23 of quantity tube 21, whole volatile organic compounds, water and carbon dioxide in sample etc. is by quantity tube 21
Capture, the 13rd interface G3 of other parts in sample from the first port 22 of quantity tube 21 into six-way valve 50, and from six
12nd interface G2 of port valve 50 is sent into the four-way valve 31 of discharger 30, and from 33 row of efferent duct with vacuum pump 34
Go out, mass flowmenter 35 monitors the delivery flow of efferent duct 33, when mass flowmenter 35, which reaches, sets flow, sample introduction knot at this time
Beam, six-way valve are closed.
4th, sample desorption：Six-way valve is closed, and inputs helium in helium input pipe 60 to six-way valve 50, and helium is from six-way valve 50
The 14th interface G4 into the 13rd interface G3, i.e. helium is blown into from the first port 22 of quantity tube 21, at this time by quantity tube
Whole volatile organic compounds, water and carbon dioxide of 21 trappings etc. are by helium from 23 row of second port of quantity tube 21
Go out, into the 16th interface G6 of six-way valve 50, and from the 16th interface G6 into the 15th interface G5, i.e., caught by quantity tube 21
Whole volatile organic compounds, water and carbon dioxide of collection etc. are transferred into cold focusing arrangement 40.
5th, the cold focusing of sample：Cold focusing arrangement 40 is opened, freezing chamber 411 of the liquid nitrogen 44 from input port 441 into housing 41
It is interior, freezing chamber 411 is cooled down, cooling temperature is can be controlled between -100 DEG C to -180 DEG C, is trapped at this time by quantity tube 21
Sample is blown by nitrogen in the first tube body 45 of cold focusing arrangement 40, and refocusing is carried out in the environment of deep cooling, is focused on and is completed
Afterwards, liquid nitrogen 44 is closed, heat gas is inputted from air inlet 461, at this time after 45 thickening of the first tube body, carbon dioxide removal
Volatile organic compounds be desorbed by the second in vivo heat gas of pipe, open gas blow pipe 48, nitrogen enters from gas blow pipe 48
The sample input 42 of first tube body 45 discharges the sample after refocusing, from the first tube body 45 out of first tube body 45
Sample output terminal 43 carries out chromatography into gas chromatograph 70.
6th, purging purification：The inlet channel 831 of sample input pipe 13 on sampling device 10 and autosampler 80 at this time
On do not take over He Suma tanks or airbag, then input nitrogen in the nitrogen input pipe 15 on the ten-way valve 12 of sampling device 10,
The nitrogen of input carries out purging purification to each interface on ten-way valve 12 and the inlet channel on autosampler 80, when six
When port valve 50 is opened, nitrogen can be to carrying out purging purification, when six-way valve 50 is closed in quantity tube 21, and nitrogen can be to discharge
Each pipeline in device 30 carries out purging purification.
The foregoing is merely a prefered embodiment of the invention, is not intended to limit the invention, it is all the present invention spirit and
All any modification, equivalent and improvement made within principle etc., should all be included in the protection scope of the present invention.
Claims (10)
1. gas concentration instrument is placed in the front end of gas chromatograph, which is characterized in that including sampling device, six-way valve, trapping dress
It puts, discharger, helium input pipe, cold focusing arrangement；
The sampling device includes sample feeding pipe；
The capturing device is quantity tube, and the quantity tube is 1/16 inch of silanization pipe, has first port and second end
Mouthful；
The discharger include four-way valve, be connected with the 18th interface of the four-way valve emptying discharge line, with it is described
The efferent duct with vacuum pump of the 19th interface connection of four-way valve；
The cold focusing arrangement has the housing of freezing chamber, and sample input and sample output terminal, institute are equipped in the housing
Sample output terminal is stated to be connected with the gas chromatograph；
11st interface of the six-way valve is connected with the sample feeding pipe of the sampling device, the 12nd interface and the discharger
Four-way valve the connection of the 17th interface, the first end of the 13rd interface of the six-way valve and the quantity tube of the capturing device
Mouth connection, the 16th interface of the six-way valve are connected with the second port of the quantity tube of the capturing device, the six-way valve
The 14th interface be connected with the helium input pipe, the sample of cold focusing arrangement is defeated described in the 15th interface of the six-way valve
Enter end connection.
2. gas concentration instrument as described in claim 1, which is characterized in that the sampling device, further include ten-way valve, automatically into
Sample device and six sample input pipes；
The first interface of the ten-way valve is connected with the input pipe of the autosampler, and second interface, the 3rd interface, the 4th connect
Mouth, the 8th interface, the 9th interface and the tenth interface are connected respectively with six sample input pipes, the 7th interface and the sample introduction
Pipe connects.
3. gas concentration instrument as described in claim 1, which is characterized in that the cold focusing arrangement, which further includes, is placed in the housing
Outer liquid nitrogen, it is described cold in the input port for being provided with to input liquid nitrogen on the housing and outlet for discharging liquid nitrogen
Freeze intracavitary and be provided with to convey the first tube body of sample and for being heated after freezing to first tube body
Second tube body, first tube body is threaded through in second tube body and bending is provided with deformation structure, positioned at the deformation
Insulation construction is provided at structure, one end of first tube body is connected with the sample input, the other end and the sample
Output terminal connects, and is respectively formed between the two ends of second tube body and first tube body and is useful for input heat gas
Air inlet and the exhaust outlet for being discharged for heat gas.
4. gas concentration instrument as described in claim 1, which is characterized in that the cold focusing arrangement further includes gas blow pipe, described
Gas blow pipe is connected with the air inlet of second tube body.
5. gas concentration instrument as claimed in claim 3, which is characterized in that first tube body is metal tube, and the second tube body is
1/8 inch of tetrafluoroethene pipe.
6. gas concentration instrument as claimed in claim 5, which is characterized in that the caliber of first tube body is less than the described second pipe
The caliber of body.
7. gas concentration instrument as described in claim 1, which is characterized in that the discharger further includes mass flowmenter, institute
Mass flowmenter is stated to be placed between the 19th interface of the four-way valve and the vacuum pump.
8. gas concentration instrument as claimed in claim 2, which is characterized in that the autosampler include free switching device and
The storage device of sample is provided for the free switching device, the free switching device includes 16 port valves and leads to described 16
The switching device that inlet channel in valve is docked with output channel, the output channel and the first interface of the ten-way valve connect
It is logical.
9. gas concentration instrument as claimed in claim 2, which is characterized in that the sampling device further includes internal standard input pipe, institute
The 5th interface for stating ten-way valve is connected with the internal standard input pipe.
10. gas concentration instrument as claimed in claim 2, which is characterized in that the sampling device further includes nitrogen input pipe, institute
The 6th interface for stating ten-way valve is connected with the nitrogen input pipe.
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| CN201711316727.0A CN108107145B (en) | 2017-12-12 | 2017-12-12 | Gas concentration instrument |
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| CN115201367A (en) * | 2022-07-11 | 2022-10-18 | 中国计量科学研究院 | Method for detecting sulfur-containing organic compounds in pollution source |
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| CN111013375A (en) * | 2019-12-30 | 2020-04-17 | 暨南大学 | CO2Absorption trap and method for improving detection peak shape of atmospheric volatile organic compound by using same |
| CN115201367A (en) * | 2022-07-11 | 2022-10-18 | 中国计量科学研究院 | Method for detecting sulfur-containing organic compounds in pollution source |
| CN115201367B (en) * | 2022-07-11 | 2024-01-26 | 中国计量科学研究院 | A method for detecting sulfur-containing organic compounds in pollution sources |
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