CN108333380A - A kind of automatic sampling apparatus and its automatic sampling method - Google Patents
A kind of automatic sampling apparatus and its automatic sampling method Download PDFInfo
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- CN108333380A CN108333380A CN201810072819.7A CN201810072819A CN108333380A CN 108333380 A CN108333380 A CN 108333380A CN 201810072819 A CN201810072819 A CN 201810072819A CN 108333380 A CN108333380 A CN 108333380A
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- 238000005070 sampling Methods 0.000 title claims abstract description 111
- 238000000034 method Methods 0.000 title claims abstract description 12
- 239000007789 gas Substances 0.000 claims abstract description 126
- 238000010926 purge Methods 0.000 claims abstract description 94
- 239000012159 carrier gas Substances 0.000 claims abstract description 88
- 230000008676 import Effects 0.000 claims abstract description 47
- 238000001514 detection method Methods 0.000 claims abstract description 29
- 238000001035 drying Methods 0.000 claims description 30
- 230000004907 flux Effects 0.000 claims description 26
- 238000000642 dynamic headspace extraction Methods 0.000 claims description 24
- 238000010438 heat treatment Methods 0.000 claims description 17
- 238000004458 analytical method Methods 0.000 claims description 14
- 239000004809 Teflon Substances 0.000 claims description 3
- 229920006362 Teflon® Polymers 0.000 claims description 3
- 238000004804 winding Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 11
- 229910052753 mercury Inorganic materials 0.000 description 11
- JJWSNOOGIUMOEE-UHFFFAOYSA-N Monomethylmercury Chemical compound [Hg]C JJWSNOOGIUMOEE-UHFFFAOYSA-N 0.000 description 9
- 238000003795 desorption Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000004587 chromatography analysis Methods 0.000 description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 3
- 230000001717 pathogenic effect Effects 0.000 description 3
- 238000005191 phase separation Methods 0.000 description 3
- 238000004227 thermal cracking Methods 0.000 description 3
- 230000004888 barrier function Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000007634 remodeling Methods 0.000 description 2
- 210000003786 sclera Anatomy 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- 235000008645 Chenopodium bonus henricus Nutrition 0.000 description 1
- 244000138502 Chenopodium bonus henricus Species 0.000 description 1
- -1 alkyl mercury Chemical compound 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 230000002000 scavenging effect Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N35/10—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices
- G01N35/1009—Characterised by arrangements for controlling the aspiration or dispense of liquids
-
- 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
- G01N30/24—Automatic injection systems
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N35/10—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices
- G01N35/1065—Multiple transfer devices
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- 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 relates to a kind of automatic sampling apparatus and its automatic sampling methods, it is characterised in that：It includes automatic alternately sampling device and first, second liang of capturing device；The automatic alternately purge gass import of sampling device, dry gas import and carrier gas inlet are connected with source purge gas, dry air source and carrier gas source respectively, two pairs of outlets of the automatic alternately sampling device are connected with first, second capturing device respectively, and the sample detection mouth of the automatic alternately sampling device is connected with detection device；Automatic alternately sampling device and first, second liang of capturing device are controlled by system, control circuit.It is the configuration of the present invention is simple, easy to operate, it can be widely applied to the analyzing processing field of sample.
Description
Technical field
The present invention relates to sample analysis process fields, more particularly to a kind of automatic sampling apparatus and its automatic sampling side
Method.
Background technology
Mercury pollution causes high risks as a kind of global contaminant to ecological environment and human health, at
For one of currently the most important Global Environmental Problems.The toxicity of mercury not fully depend on total amount, and with its existing forms and ring
Border behavior is closely related.In mercury cycle, mercury is existing for variform, substantially to there is 3 kinds of forms:Element mercury, inorganic mercury
And organic mercury.Methyl mercury is the maximum organic mercury form of toxicity, has been cited as in international chemical Material Safety program and most endangers for 6 kinds
One of the substance of danger.Due to the significant damage of methyl mercury, in recent years, methyl mercury in related water quality, soil, air and aquatic products
Analysis be increasingly becoming research hotspot, the means for detecting methyl mercury are also growing.
There are many method for measuring methyl mercury at present, and gas chromatography can measure alkyl mercury, and appearance is very fast, but ECD detectors
It is not strong to detect mercury specificity, impurity interference is big.High performance liquid chromatography is also used for the analysis of mercury, and coexisting ion interference is less, but
The disadvantage that there is also detector specificities is not strong, the analysis linearity is bad.Compared with preceding two quasi-instruments technology, atomic emission spectrum
Instrument sensitivity higher, by spectral line and matrix interference it is lower compared with smaller, detection limit, therefore with this method detection methyl mercury the most at
It is ripe reliable.Currently, the mercury morphological analysis method for being widely recognized as and being applied in the world --- U.S. EPA 1630 is exactly foundation
Detector detection.
The Chinese patent of Patent No. 2015101264393 discloses a kind of " methyl mercury thermal desorption sampling device ", including
Walk flowmeter, heating coil, heating power supply, heater switch, heating power supply voltage regulator.The sampling device can only be to methyl mercury
The tenax adsorption tubes of enriched completion carry out Thermal desorption sampling step, can not carry out tenax adsorption tube methyl mercuries enrichment step
Suddenly, the not full-automatic methyl sclera remodeling sampling device in complete meaning；And channel is unique, can only sequence sample introduction, sample treatment
Efficiency is low.Overseas market has a full-automatic methyl mercury analyzer, but when in face of domestic market, due to technical barrier and costliness
Instrument expense, greatly hinder demand of the domestic consumer to methyl sclera remodeling.
Invention content
In view of the above-mentioned problems, the object of the present invention is to provide one kind effectively shorten sample purge trapping, Thermal desorption, sample introduction when
Between, improve the automatic sampling apparatus and its automatic sampling method of sample determination efficiency.
To achieve the above object, the present invention takes following technical scheme：A kind of automatic sampling apparatus, it is characterised in that：Its
Including replacing sampling device and first, second liang of capturing device automatically；The automatic alternately purge gass import of sampling device,
Dry gas import and carrier gas inlet are connected with source purge gas, dry air source and carrier gas source respectively, the automatic alternately sampling device
Two pairs of outlets be connected respectively with first, second capturing device, it is described it is automatic alternately sampling device sample detection mouth
It is connected with detection device；Automatic alternately sampling device and first, second liang of capturing device are controlled by system, control circuit.
The automatic alternately sampling device includes the first~the 4th solenoid valve and the first~the 4th triple valve；Described first
Solenoid valve and the COM port of second solenoid valve are separately connected described as first pair of outlet of the automatic alternately sampling device
The both ends of second capturing device；The COM port of the third solenoid valve and the 4th solenoid valve is as the automatic alternately sample introduction dress
The second pair of outlet set is separately connected the both ends of first capturing device；The normally open end of first solenoid valve and described
The normal-closed end of four solenoid valves is connected by first triple valve, another interface of first triple valve as carrier gas inlet with
Carrier gas source is connected；The normally open end of the normal-closed end of first solenoid valve and the 4th solenoid valve is connected by second triple valve
It connects, another interface of second triple valve is as the automatic drying gas import for replacing sampling device；Second electromagnetism
The normally open end of valve is connected with the normal-closed end of the third solenoid valve by the third triple valve, the third triple valve it is another
Sample detection mouth of the interface as the automatic alternately sampling device；The normal-closed end of the second solenoid valve and the third electromagnetism
The normally open end of valve is connected by the 4th triple valve, and another interface of the 4th triple valve is as the automatic alternately sample introduction
The purge gass import of device；Each solenoid valve is connected with system, control circuit, is controlled by the system, control circuit.
The first, second capturing device structure is identical, first, second capturing device include a trap tube, with
The trap tube connected heating module and refrigerating module；The heating module and refrigerating module with system, control circuit phase
Even, it is controlled by the system, control circuit.
The heating module uses fan coolling module using winding resistive heating module, the refrigerating module.
The automatic alternately purge gass import of sampling device and dry gas import respectively by purge gass connection component and
Dry gas connection component is connected with purge gas source and dry gas source, and the carrier gas inlet of the automatic alternately sampling device passes through
Carrier gas connection component is connected with gas of carrier gas source.
The purge gass connection component includes purge stream gauge, purge gass flow control valve and sample introduction needle；It is described to blow
Scavenging flowmeter bottom side is connected with purge gas source outlet, and the pipe between the purge stream gauge and purge gas source
The purge gass flow control valve is arranged in road, and purge stream gauge top is connected with sample introduction needle side interface,
Interface is connected with the automatic purge gass import for replacing sampling device above the sample introduction needle, and syringe needle is inserted below the sample introduction needle
Enter into sample bottle.
The dry gas connection component includes dry gas stream gauge, dry gas stream amount control valve and valve, described dry
The outlet of pathogenic dryness flowmeter bottom and dry gas source is connected, and dry gas stream gauge top automatic replaces sampling device with described
Carrier gas inlet be connected, and the dry gas stream amount control is set on the pipeline between the dry gas stream gauge and dry gas source
Valve processed, on the pipeline between the dry gas stream gauge and the automatic drying gas import for replacing sampling device described in setting
Valve.
The carrier gas connection component includes carrier gas flux meter and carrier gas flux control valve, carrier gas flux meter bottom with
The outlet of gas of carrier gas source is connected, and top is connected with the automatic carrier gas inlet for replacing sampling device, the carrier gas flux control
Valve processed is arranged on the pipeline between the carrier gas flux meter and gas of carrier gas source.
The automatic alternately sampling device and first, second capturing device, purge gas source, dry gas source, load
1/8 Teflon piping connection is all made of between gas gas source.
A kind of automatic sampling method of automatic sampling apparatus, it is characterised in that include the following steps：
1) instrument ready state：Purge gass flow control valve and dry gas stream amount control valve are closed, and opens carrier gas
Flow control valve, while the trap tube in two capturing devices does not work, carrier gas by replace automatically the carrier gas of sampling device into
Mouth enters enters detection device after the trap tube of the second capturing device；
2) the purge and trap state of the first capturing device：It keeps carrier gas flux control valve constant, opens purge gass flow
Control valve, while the trap tube work in the first capturing device, enter the purge gass import by replacing sampling device automatically
Sample trapped；
3) drying regime of the first capturing device：It after the completion of purge and trap, keeps carrier gas flux control valve constant, closes
Purge gass flow control valve, and open dry gas stream amount control valve, dry gas by replacing the drying gas of sampling device automatically
Import enters the sample trapped to the first capturing device and is dried；
4) analysis state of the first capturing device：After the completion of drying, auto-changeover control is filled by system, control circuit
Each solenoid valve in setting carries out Vavle switching, simultaneously closes off purge gass flow control valve and dry gas stream amount control valve, opens
Carrier gas flux control valve, carrier gas drive the sample after the parsing of the first capturing device to be examined by the sample for replacing sampling device automatically
Mouth is surveyed to be detected into detection device；
5) the purge and trap state of the second capturing device：In first capturing device resolving, purge gass flow control is opened
Valve processed, closes dry gas stream amount control valve, and purge gass are caught by the purge gass import for replacing sampling device automatically into second
Trap tube in acquisition means carries out purge and trap；
6) drying regime of the second capturing device：After the completion of second capturing device purge and trap, purge gass flow control is closed
Valve processed, opens dry gas stream amount control valve, and dry gas is caught by the drying gas import for replacing sampling device automatically into second
Acquisition means are dried；
7) analysis state of the second capturing device：After the completion of the drying of second capturing device, system, control circuit carries out valve and cuts
It changes so that carrier gas enters the second capturing device by carrier gas inlet, and the sample in the second capturing device is driven to enter subsequent detection dress
It sets；
8) step 2)~7 are repeated) so that sample alternately enters first, second liang of capturing device and carries out purge and trap reconciliation
Analysis, and then enter detection device.
The invention adopts the above technical scheme, which has the following advantages：1, replace sampling device in the present invention automatically
There are two injection ports for middle setting, are switched over by the port to solenoid valve, can form two non-interfering sample intake passages, can
It is respectively used to purge and trap or sample introduction, effectively shorten sample effectively shortens sample purge trapping, Thermal desorption, sample injection time,
Meets the needs of client measures batch samples.2, the present invention due to replace automatically sampling device using conventional solenoid valve and
Triple valve is attached, capturing device use heating module and refrigerating module be conventional equipment, effectively reduce operation at
This, while breaking the dual barrier of external import instrument price and technical monopoly.Thus, the present invention can be widely applied to sample
Analysis field.
Description of the drawings
Fig. 1 is schematic structural view of the invention；
Fig. 2 is automatic alternately sampling device structural schematic diagram of the invention；
Fig. 3 is that instrument ready state of the present invention and the first capturing device enter purge and trap status diagram；
Fig. 4 is that the first capturing device of the invention enters drying regime schematic diagram；
Fig. 5 is that the first capturing device of the invention enters analysis state schematic diagram.
Specific implementation mode
The present invention is described in detail below with reference to the accompanying drawings and embodiments.It should be appreciated, however, that the offer of attached drawing is only
For a better understanding of the present invention, they should not be interpreted as limitation of the present invention.In the description of the present invention, it is to be understood that
, term " first ", " second " etc. are only used for the purpose of description, are not understood to indicate or imply relatively important
Property.
As shown in Figure 1, a kind of automatic sampling apparatus provided by the invention comprising automatic alternately sampling device 1 and the
One, second liang of capturing device 2,3.The automatic alternately purge gass import of sampling device 1, dry gas import and carrier gas inlet (are schemed
In b mouths, d mouthfuls and a mouthfuls) be connected respectively with source purge gas, dry air source and carrier gas source, replace two couple of sampling device 1 automatically
Outlet is connected with the first, second capturing device 2,3 respectively, the sample detection mouth (i.e. c mouthfuls in figure) of automatic alternately sampling device 1
It is connected with detection device, detection device includes gas phase separation chromatography column 4 (GC), thermal cracking pipe 5 and detector 6.Wherein, automatically
Alternately sampling device 1 and first, second liang of capturing device 2,3 are controlled by system, control circuit.
As shown in Fig. 2, alternately sampling device 1 includes the first~the 4th solenoid valve V1~V4 and the first~the 4th 3 automatically
The first couple of the COM port of port valve T1~T4, the first solenoid valve V1 and second solenoid valve V2 as automatic alternately sampling device 1
Outlet is separately connected the both ends of the second capturing device 3；The COM port of third solenoid valve V3 and the 4th solenoid valve V4 are used as certainly
Second pair of outlet of dynamic alternately sampling device 1 is separately connected the both ends of the first capturing device 2；The normally open end of first solenoid valve V1
(ends NO) is connected with the normal-closed end (ends NC) of the 4th solenoid valve V4 by the first triple valve T1, and first the another of triple valve T1 connects
Mouth is connected as carrier gas inlet (i.e. a mouthfuls) with carrier gas source；The normal-closed end (ends NC) of first solenoid valve V1 and the 4th solenoid valve V4's
Normally open end (ends NO) is by the second triple valve T2 connections, and another interface of the second triple valve T2 is as automatic alternately sampling device 1
Drying gas import (i.e. d mouthfuls)；The normally open end (ends NO) of second solenoid valve V2 and the normal-closed end (ends NC) of third solenoid valve V3 are logical
The T3 connections of third triple valve are crossed, another interface of third triple valve T3 is as the automatic sample detection mouth for replacing sampling device 1
(i.e. c mouthfuls)；The normal-closed end (ends NC) of second solenoid valve V2 passes through the 4th triple valve with the normally open end (ends NO) of third solenoid valve V3
T4 is connected, and another interface of the 4th triple valve T4 is as purge gass import (i.e. b mouthfuls).Each solenoid valve V1~V4 is controlled with system
Circuit is connected, and is controlled by system, control circuit.
First, second capturing device 2,3 structures are identical, and the present invention is introduced by taking the first capturing device 2 as an example, the trapping
Device includes trap tube 21 (31), the heating module being connected with trap tube 21 (31) 22 (32) and refrigerating module 22 (33).Wherein,
Heating module 22 (32) and refrigerating module 23 (33) are connected with system, control circuit, are controlled by system, control circuit.
Automatically alternately the purge gass import of sampling device 1 and dry gas import by purge gass connection component 7 and are done respectively
Pathogenic dryness connection component 8 is connected with purge gas source and dry gas source.Wherein, purge gass connection component 7 includes purge gass flow
Meter 71, purge gass flow control valve 72 and sample introduction needle 73.71 bottom side of purge stream gauge exports phase with purge gas source
Even, and on the pipeline between purge stream gauge 71 and purge gas source purge gass flow control valve 72, purge stream are set
The 71 top other side of gauge is connected with 73 side interface of sample introduction needle, 73 top interface of sample introduction needle with replace sampling device 1 automatically
(b mouthfuls) of purge gass import is connected, and 73 lower section syringe needle of sample introduction needle is inserted into sample bottle.Dry gas connection component 8 includes dry gas
Flowmeter 81, dry gas stream amount control valve 82 and valve 83,81 bottom of dry gas stream gauge export phase with dry gas source
Even, 81 top of dry gas stream gauge is connected with the automatic carrier gas inlet for replacing sampling device 1, and dry gas stream gauge 81 and drying
Dry gas stream amount control valve 82 is set on the pipeline between gas source, and dry gas stream gauge replaces the dry of sampling device with automatic
Valve 83 is set on the pipeline between pathogenic dryness import (d mouthfuls).
It is automatic to be alternately connected by carrier gas connection component 9 between the carrier gas inlet and gas of carrier gas source of sampling device 1, the load
Gas connection component 9 includes carrier gas flux meter 91 and carrier gas flux control valve 92,91 bottom of carrier gas flux meter and gas of carrier gas source
Outlet is connected, and top is connected with the automatic carrier gas inlet (a mouthfuls) for replacing sampling device 1, and carrier gas flux control valve 92 is arranged
On pipeline between carrier gas flux meter 91 and gas of carrier gas source.
As a preferred embodiment, automatic alternately sampling device 1 and the first, second capturing device 2,3, purge gas
1/8 Teflon piping connection is all made of between source, dry gas source, gas of carrier gas source.
As a preferred embodiment, the heating module in two capturing devices uses winding resistive heating module.
As a preferred embodiment, the refrigerating module in two capturing devices uses fan coolling module.
As shown in Fig. 3~Fig. 5, it is based on above-mentioned automatic sampling apparatus, the present invention also provides a kind of automatic sampling methods, including
Following steps：
1) instrument ready state：Purge gass flow control valve 72 and dry gas stream amount control valve 82 are closed, and is opened
Carrier gas flux control valve 92, while the trap tube in two capturing devices 2,3 does not work, carrier gas by replacing sampling device automatically
1 carrier gas inlet enters detection device after the trap tube of the second capturing device 3.
At this point, the tenax trap tubes in two capturing devices are in off position, purge gass flow control valve 72,
Dry gas stream amount control valve 82 is closed, and carrier gas flux control valve 92 is opened, and gas of carrier gas enters solenoid valve by carrier gas inlet
The ends NO of V1, and flowed out by the ends COM of solenoid valve V1, by entering electricity after the tenax trap tubes 31 in the second capturing device 3
The ends COM of magnet valve V2, and flowed out by the ends NO of solenoid valve V2, sample port c enters gas phase separation chromatography column 4, thermal cracking after testing
Pipe 5 and detector 6.
2) the purge and trap state of the first capturing device 2：It keeps carrier gas flux control valve 92 constant, opens purge stream
Control valve door 72, while the trap tube 21 in the first capturing device 2 works, to the purge gass by replacing sampling device 1 automatically
The sample that import enters is trapped.
As shown in figure 3, the present invention is introduced so that the first capturing device 2 initially enters working condition as an example.Purge and trap
When, carrier gas is run still according to instrument ready state；Purge gass flow control valve 72 is opened, and purge gass pass through sample introduction needle and sample
After product bottle, automatic alternately sampling device 1, purge gas are entered by purge gass import and enter the ends NO of solenoid valve V3, and by electromagnetism
After the ends the COM outflow of valve V3, into solenoid valve V4's after the tenax trap tubes 21 in the first capturing device 2 trap sample
The ends COM are expelled to valve 83 through dry gas import, are discharged into discarded collection device after the normally open end outflow of solenoid valve V4.
3) drying regime of the first capturing device 2：After the completion of purge and trap, keep carrier gas flux control valve 92 constant,
Purge gass flow control valve 72 is closed, and opens dry gas stream amount control valve 82, dry gas by replacing sampling device 1 automatically
Drying gas import enter the sample that is trapped to the first capturing device 2 and be dried.
As shown in figure 4, when dry, carrier gas is run still according to instrument ready state；Dry gas stream amount control valve 82 is beaten
It opens, dry gas enters automatic alternately sampling device 1 by drying gas import, and dry gas is flowed into from the normally open end of solenoid valve V4, warp
The ends COM of solenoid valve V4 enter the first capturing device 2, and enter the COM of solenoid valve V3 after being flowed out by 2 upper end of the first capturing device
End is flowed out by the normally open end of solenoid valve V3 be expelled to the sample introduction needle 73 in purge gass connection component 7 through purge gass import later, by
The middle part of sample introduction needle 73 is discharged.
4) analysis state of the first capturing device 2：After the completion of drying, auto-changeover control is filled by system, control circuit
Each solenoid valve in setting carries out Vavle switching, simultaneously closes off purge gass flow control valve 72 and dry gas stream amount control valve 82,
Carrier gas flux control valve 92 is opened, carrier gas drives the sample after the parsing of the first capturing device 2 by replacing sampling device automatically
Sample detection mouth be detected into detection device.
As shown in figure 5, when the first capturing device parses, 4 solenoid valve V1~V4 progress valves are controlled by circuit system and are cut
It changes so that the ends NO of each solenoid valve are closed, and the ends NC are opened, and purge gass flow control valve 72 and dry gas stream amount control are simultaneously closed off
Valve 82 processed opens carrier gas flux control valve 92.Specific work process is：Gas of carrier gas is flowed by the ends NC of solenoid valve V4,
And flowed out by the ends COM of solenoid valve V4, entered by the lower end of the tenax trap tubes in the first capturing device, while heating module
Work, the gas after parsing enter the ends COM of solenoid valve V3, and are flowed out by the ends NC of solenoid valve V3, through sample detection mouth c into
Enter gas phase separation chromatography column, thermal cracking pipe and detector.
5) the purge and trap state of the second capturing device 3：In first capturing device, 2 resolving, purge gass flow is opened
Control valve 72, closes dry gas stream amount control valve 82, and purge gass are entered by the purge gass import for replacing sampling device 1 automatically
Trap tube 31 in second capturing device 3 carries out purge and trap.
In 2 resolving of the first capturing device, the tenax trap tubes 31 in the second capturing device 3 may be at ready
State or purge and trap or drying regime (binary channels replaces sample introduction effect).When in purge and trap state, purge gass flow
Control valve 72 is opened, and purge gass enter automatic alternately sampling device 1 through purge gass import, into the ends NC of solenoid valve V2, and
It is flowed out by the ends COM of solenoid valve V2, the ends COM of solenoid valve V1 is entered after the tenax trap tubes 31 in the second capturing device 3,
And after being flowed out by the ends NC of solenoid valve V1, it is expelled to valve 83 through dry gas import, is then discharged into discarded collection device.
6) drying regime of the second capturing device 3：After the completion of second capturing device, 3 purge and trap, purge gass flow is closed
Control valve 72, opens dry gas stream amount control valve 82, and dry gas is entered by the drying gas import for replacing sampling device automatically
Second capturing device is dried.
When in drying regime, dry gas stream amount control valve 82 is opened, and dry gas enters automatic hand over by drying gas import
For sampling device 1, the normal-closed end that dry gas enters solenoid valve V1 flows into, and the ends COM through solenoid valve V1 enter the second trapping and fill
3 are set, and enters the ends COM of solenoid valve V2 after being flowed out by 3 upper end of the second capturing device, is flowed out later by the normal-closed end of solenoid valve V2
It is expelled to the sample introduction needle 73 in purge gass connection component 7 through purge gass import, is discharged by the middle part of sample introduction needle 73.
7) analysis state of the second capturing device 3：After the completion of the drying of second capturing device 3, system, control circuit carries out valve
Switching so that carrier gas enters the second capturing device 3 by carrier gas inlet, and the sample in the second capturing device 3 is driven to enter follow-up inspection
Survey device.
8) step 2)~7 are repeated) so that sample alternately enter first, second liang of capturing device 2,3 carry out purge and trap and
Parsing, and then enter detection device.Reach binary channels alternating sample introduction effect, the purge and trap stand-by period is greatly saved, carries
High instrument working efficiency.
The various embodiments described above are merely to illustrate the present invention, wherein the structure of each component, connection type and manufacture craft etc. are all
It can be varied from, every equivalents carried out based on the technical solution of the present invention and improvement should not exclude
Except protection scope of the present invention.
Claims (10)
1. a kind of automatic sampling apparatus, it is characterised in that：It includes automatic alternately sampling device and first, second liang of trapping dress
It sets；The automatic alternately purge gass import of sampling device, dry gas import and carrier gas inlet respectively with source purge gas, dry gas
Source is connected with carrier gas source, it is described it is automatic alternately sampling device two pairs of outlets respectively with the first, second capturing device phase
Even, the sample detection mouth of the automatic alternately sampling device is connected with detection device；It is described it is automatic alternately sampling device and first,
Second liang of capturing device is controlled by system, control circuit.
2. a kind of automatic sampling apparatus as described in claim 1, it is characterised in that：The automatic alternately sampling device includes the
One~the 4th solenoid valve and the first~the 4th triple valve；
The first pair of outlet of first solenoid valve and the COM port of second solenoid valve as the automatic alternately sampling device
It is separately connected the both ends of second capturing device；
Second pair outlet of the COM port of the third solenoid valve and the 4th solenoid valve as the automatic alternately sampling device
It is separately connected the both ends of first capturing device；
The normally open end of first solenoid valve is connected with the normal-closed end of the 4th solenoid valve by first triple valve, described
Another interface of first triple valve is connected as carrier gas inlet with carrier gas source；
The normal-closed end of first solenoid valve is connected with the normally open end of the 4th solenoid valve by second triple valve, described
Drying gas import of another interface of second triple valve as the automatic alternately sampling device；
The normally open end of the second solenoid valve is connected with the normal-closed end of the third solenoid valve by the third triple valve, described
Sample detection mouth of another interface of third triple valve as the automatic alternately sampling device；
The normal-closed end of the second solenoid valve is connected with the normally open end of the third solenoid valve by the 4th triple valve, described
Purge gass import of another interface of 4th triple valve as the automatic alternately sampling device；
Each solenoid valve is connected with system, control circuit, is controlled by the system, control circuit.
3. a kind of automatic sampling apparatus as described in claim 1, it is characterised in that：The first, second capturing device structure
Identical, first, second capturing device includes a trap tube, the heating module being connected with the trap tube and cooling mould
Block；The heating module and refrigerating module are connected with system, control circuit, are controlled by the system, control circuit.
4. a kind of automatic sampling apparatus as claimed in claim 3, it is characterised in that：The heating module is using winding resistance-type
Heating module, the refrigerating module use fan coolling module.
5. a kind of automatic sampling apparatus as described in claim 1, it is characterised in that：The purging of the automatic alternately sampling device
Gas import and dry gas import pass through purge gass connection component and dry gas connection component and purge gas source and dry gas respectively
Body source is connected, and the carrier gas inlet of the automatic alternately sampling device is connected by carrier gas connection component with gas of carrier gas source.
6. a kind of automatic sampling apparatus as claimed in claim 5, it is characterised in that：The purge gass connection component includes purging
Air-flow gauge, purge gass flow control valve and sample introduction needle；The purge stream gauge bottom side is exported with purge gas source
It is connected, and the purge gass flow control valve, institute is set on the pipeline between the purge stream gauge and purge gas source
Purge stream gauge top is stated with sample introduction needle side interface to be connected, above the sample introduction needle interface with it is described it is automatic replace into
The purge gass import of sampling device is connected, and syringe needle is inserted into sample bottle below the sample introduction needle.
7. a kind of automatic sampling apparatus as claimed in claim 5, it is characterised in that：The dry gas connection component includes drying
Air-flow gauge, dry gas stream amount control valve and valve, dry gas stream gauge bottom are connected with dry gas source outlet,
Dry gas stream gauge top and the automatic carrier gas inlet for replacing sampling device are connected, and the dry gas stream gauge with
The dry gas stream amount control valve, the dry gas stream gauge and the automatic friendship are set on the pipeline between dry gas source
For the valve is arranged on the pipeline between the drying gas import of sampling device.
8. a kind of automatic sampling apparatus as claimed in claim 5, it is characterised in that：The carrier gas connection component includes carrier gas stream
Gauge and carrier gas flux control valve, the outlet of carrier gas flux meter bottom and gas of carrier gas source are connected, top with it is described automatically
Alternately the carrier gas inlet of sampling device is connected, and the carrier gas flux control valve is arranged in the carrier gas flux meter and carrier gas gas
On pipeline between body source.
9. a kind of automatic sampling apparatus as described in claim 1, it is characterised in that：It is described it is automatic alternately sampling device with it is described
1/8 Teflon pipeline company is all made of between first, second capturing device, purge gas source, dry gas source, gas of carrier gas source
It connects.
10. a kind of automatic sampling method using such as any one of claim 1~9 described device, it is characterised in that including following
Step：
1) instrument ready state：Purge gass flow control valve and dry gas stream amount control valve are closed, and opens carrier gas flux
Control valve, while the trap tube in two capturing devices does not work, carrier gas by replace automatically the carrier gas inlet of sampling device into
Enter and enters detection device after the trap tube of the second capturing device；
2) the purge and trap state of the first capturing device：It keeps carrier gas flux control valve constant, opens purge gass flow control
Valve, while the trap tube work in the first capturing device, to the sample entered by the purge gass import for replacing sampling device automatically
Product are trapped；
3) drying regime of the first capturing device：It after the completion of purge and trap, keeps carrier gas flux control valve constant, closes purging
Flow control valves door, and dry gas stream amount control valve is opened, dry gas is by the alternately drying gas import of sampling device automatically
It is dried into the sample trapped to the first capturing device；
4) analysis state of the first capturing device：After the completion of drying, by system, control circuit in automatic switching control device
Each solenoid valve carry out Vavle switching, simultaneously close off purge gass flow control valve and dry gas stream amount control valve, open carrier gas
Flow control valve, carrier gas drive through the first capturing device parsing after sample by automatically replace sampling device sample detection mouth
It is detected into detection device；
5) the purge and trap state of the second capturing device：In first capturing device resolving, purge stream control valve is opened
Door, closes dry gas stream amount control valve, and purge gass enter the second trapping by the purge gass import for replacing sampling device automatically and fill
Trap tube in setting carries out purge and trap；
6) drying regime of the second capturing device：After the completion of second capturing device purge and trap, purge stream control valve is closed
Door, opens dry gas stream amount control valve, and dry gas enters the second trapping by the drying gas import for replacing sampling device automatically and fills
It sets and is dried；
7) analysis state of the second capturing device：After the completion of the drying of second capturing device, system, control circuit carries out Vavle switching, makes
It obtains carrier gas and the second capturing device is entered by carrier gas inlet, the sample in the second capturing device is driven to enter subsequent detection device；
8) step 2)~7 are repeated) so that sample alternately enters first, second liang of capturing device and carries out purge and trap and parsing, into
And enter detection device.
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