CN108333380B - Automatic sample injection device and automatic sample injection method thereof - Google Patents
Automatic sample injection device and automatic sample injection method thereof Download PDFInfo
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- CN108333380B CN108333380B CN201810072819.7A CN201810072819A CN108333380B CN 108333380 B CN108333380 B CN 108333380B CN 201810072819 A CN201810072819 A CN 201810072819A CN 108333380 B CN108333380 B CN 108333380B
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- 238000002347 injection Methods 0.000 title claims abstract description 117
- 239000007924 injection Substances 0.000 title claims abstract description 117
- 238000000034 method Methods 0.000 title claims abstract description 16
- 239000007789 gas Substances 0.000 claims abstract description 141
- 238000010926 purge Methods 0.000 claims abstract description 105
- 239000012159 carrier gas Substances 0.000 claims abstract description 90
- 238000001514 detection method Methods 0.000 claims abstract description 32
- 238000004458 analytical method Methods 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims description 60
- 238000010438 heat treatment Methods 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 13
- 230000008569 process Effects 0.000 claims description 5
- 238000007664 blowing Methods 0.000 claims description 4
- 239000004809 Teflon Substances 0.000 claims description 3
- 229920006362 Teflon® Polymers 0.000 claims description 3
- 238000005070 sampling Methods 0.000 claims description 3
- 238000004804 winding Methods 0.000 claims description 2
- JJWSNOOGIUMOEE-UHFFFAOYSA-N Monomethylmercury Chemical compound [Hg]C JJWSNOOGIUMOEE-UHFFFAOYSA-N 0.000 description 12
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 10
- 229910052753 mercury Inorganic materials 0.000 description 10
- 238000002076 thermal analysis method Methods 0.000 description 4
- 238000000926 separation method Methods 0.000 description 3
- 238000004227 thermal cracking Methods 0.000 description 3
- 230000004888 barrier function Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 101100204059 Caenorhabditis elegans trap-2 gene Proteins 0.000 description 1
- -1 alkyl mercury Chemical compound 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 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
- 230000008676 import Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003562 morphometric effect Effects 0.000 description 1
- 238000013425 morphometry Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 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
- 238000012360 testing method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- 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 invention relates to an automatic sample injection device and an automatic sample injection method thereof, which are characterized in that: the device comprises an automatic alternating sample injection device, a first trapping device and a second trapping device; the purge gas inlet, the dry gas inlet and the carrier gas inlet of the automatic alternating sample injection device are respectively connected with a purge gas source, a dry gas source and a carrier gas source, two pairs of sample outlets of the automatic alternating sample injection device are respectively connected with the first trapping device and the second trapping device, and a sample detection port of the automatic alternating sample injection device is connected with the detection device; the automatic alternating sample injection device, the first trapping device and the second trapping device are controlled by a system control circuit. The invention has simple structure and convenient operation, and can be widely applied to the field of analysis and treatment of samples.
Description
Technical Field
The invention relates to the field of sample analysis and processing, in particular to an automatic sample injection device and an automatic sample injection method thereof.
Background
Mercury pollution, a global pollutant, has posed a great hazard to the ecological environment and human health, and is currently one of the most important global environmental problems. The toxicity of mercury is not entirely dependent on the total amount, but is closely related to its morphology and environmental behavior. In the mercury cycle, mercury exists in a variety of forms, essentially 3 forms, elemental mercury, inorganic mercury, and organic mercury. Methylmercury is the most toxic form of organomercury and has been listed as one of the 6 most dangerous substances in the international chemical safety program. Due to the huge harm of methyl mercury, in recent years, analysis of the methyl mercury in water quality, soil, air and aquatic products is becoming a research hot spot, and means for detecting the methyl mercury are also being developed.
At present, a plurality of methods for measuring methyl mercury are available, the gas chromatography can be used for measuring alkyl mercury, the peak is rapid, but the specificity of mercury detection by an ECD detector is not strong, and the impurity interference is large. High performance liquid chromatography is also used for mercury analysis, and has the defects of low detector specificity and poor analysis linearity, although the co-existence ion interference is less. Compared with the prior two instrument technologies, the atomic emission spectrometer has higher sensitivity, smaller interference caused by spectral lines and matrixes and lower detection limit, so that the method for detecting the methylmercury is most mature and reliable. Currently, the mercury morphometric method, us EPA 1630, is widely accepted and practiced internationally, and is based on this detector.
The Chinese patent with the patent number 2015101264393 discloses a methyl mercury thermal analysis sample injection device which comprises a step flow meter, a heating coil, a heating power supply, a heating switch and a heating power supply voltage regulator. The sample injection device can only carry out a thermal analysis sample injection step on the tenax adsorption tube after the enrichment of the methyl mercury is completed, but can not carry out the enrichment step of the methyl mercury of the tenax adsorption tube, and is not a full-automatic methyl mercury determination sample injection device in a complete sense; and the channel is unique, only sequential sample injection is performed, and the sample treatment efficiency is low. The foreign market has a full-automatic methylmercury tester, but when facing the domestic market, the requirements of domestic consumers on methylmercury testing are greatly hindered due to technical barriers and expensive instrument cost.
Disclosure of Invention
Aiming at the problems, the invention aims to provide an automatic sample injection device and an automatic sample injection method thereof, which can effectively shorten the time of sample purging, trapping, thermal analysis and sample injection and improve the sample measurement efficiency.
In order to achieve the above purpose, the present invention adopts the following technical scheme: an automatic sampling device, its characterized in that: the device comprises an automatic alternating sample injection device, a first trapping device and a second trapping device; the purge gas inlet, the dry gas inlet and the carrier gas inlet of the automatic alternating sample injection device are respectively connected with a purge gas source, a dry gas source and a carrier gas source, two pairs of sample outlets of the automatic alternating sample injection device are respectively connected with the first trapping device and the second trapping device, and a sample detection port of the automatic alternating sample injection device is connected with the detection device; the automatic alternating sample injection device, the first trapping device and the second trapping device are controlled by a system control circuit.
The automatic alternating sample injection device comprises first to fourth electromagnetic valves and first to fourth three-way valves; the COM ports of the first electromagnetic valve and the second electromagnetic valve are used as a first pair of sample outlets of the automatic alternating sample injection device and are respectively connected with two ends of the second trapping device; the COM ports of the third electromagnetic valve and the fourth electromagnetic valve are used as second pairs of sample outlets of the automatic alternating sample injection device and are respectively connected with two ends of the first trapping device; the normally-open end of the first electromagnetic valve is connected with the normally-closed end of the fourth electromagnetic valve through the first three-way valve, and the other interface of the first three-way valve is used as a carrier gas inlet to be connected with a carrier gas source; the normally closed end of the first electromagnetic valve and the normally open end of the fourth electromagnetic valve are connected through the second three-way valve, and the other interface of the second three-way valve is used as a dry gas inlet of the automatic alternating sample injection device; the normal open end of the second electromagnetic valve is connected with the normal closed end of the third electromagnetic valve through the third three-way valve, and the other interface of the third three-way valve is used as a sample detection port of the automatic alternating sample injection device; the normally closed end of the second electromagnetic valve is connected with the normally open end of the third electromagnetic valve through the fourth three-way valve, and the other interface of the fourth three-way valve is used as a purge gas inlet of the automatic alternating sample injection device; each electromagnetic valve is connected with a system control circuit and is controlled by the system control circuit.
The first trapping device and the second trapping device have the same structure, and each of the first trapping device and the second trapping device comprises a trapping pipe, a heating module and a cooling module which are connected with the trapping pipe; the heating module and the cooling module are both connected with the system control circuit and controlled by the system control circuit.
The heating module adopts a winding resistance type heating module, and the cooling module adopts a fan cooling module.
The automatic alternating sample injection device comprises a blowing gas inlet, a drying gas inlet, a blowing gas connecting assembly, a drying gas connecting assembly, a carrier gas inlet, a carrier gas connecting assembly and a carrier gas source.
The purge gas connecting component comprises a purge gas flowmeter, a purge gas flow control valve and a sample injection needle; one side of the bottom of the purging airflow meter is connected with a purging gas source outlet, a purging airflow control valve is arranged on a pipeline between the purging airflow meter and the purging gas source, the upper part of the purging airflow meter is connected with a lateral interface of a sample injection needle, the interface above the sample injection needle is connected with a purging gas inlet of the automatic alternating sample injection device, and a needle below the sample injection needle is inserted into a sample bottle.
The drying gas connecting assembly comprises a drying gas flowmeter, a drying gas flow control valve and a valve, wherein the bottom of the drying gas flowmeter is connected with a drying gas source outlet, the upper part of the drying gas flowmeter is connected with a carrier gas inlet of the automatic alternating sample injection device, the drying gas flow control valve is arranged on a pipeline between the drying gas flowmeter and the drying gas source, and the valve is arranged on a pipeline between the drying gas flowmeter and the drying gas inlet of the automatic alternating sample injection device.
The carrier gas connecting assembly comprises a carrier gas flowmeter and a carrier gas flow control valve, the bottom of the carrier gas flowmeter is connected with a carrier gas source outlet, the upper part of the carrier gas flowmeter is communicated with a carrier gas inlet of the automatic alternating sample injection device, and the carrier gas flow control valve is arranged on a pipeline between the carrier gas flowmeter and the carrier gas source.
The automatic alternating sample injection device is connected with the first trapping device, the second trapping device, the purging gas source, the drying gas source and the carrier gas source through 1/8 Teflon pipelines.
An automatic sample feeding method of an automatic sample feeding device is characterized by comprising the following steps:
1) Instrument ready state: closing a purging air flow control valve and a drying air flow control valve, opening a carrier gas flow control valve, enabling the collecting pipes in the two collecting devices to be inoperative, and enabling carrier gas to enter the detecting device through the carrier gas inlet of the automatic alternating sample feeding device after entering the collecting pipe of the second collecting device;
2) Purge-trap state of the first trap: keeping the carrier gas flow control valve unchanged, opening the purge gas flow control valve, and simultaneously, working a trapping pipe in the first trapping device to trap a sample entering from a purge gas inlet of the automatic alternating sample injection device;
3) Dry state of the first trapping device: after purging and trapping are completed, keeping the carrier gas flow control valve unchanged, closing the purging air flow control valve, and opening the drying air flow control valve, wherein the drying air enters a drying air inlet of the automatic alternating sample injection device to dry the sample trapped by the first trapping device;
4) Analysis state of the first trapping device: after the drying is finished, valve switching is carried out on all electromagnetic valves in the automatic switching control device through a system control circuit, meanwhile, a purging airflow control valve and a drying airflow control valve are closed, a carrier gas flow control valve is opened, and the carrier gas drives a sample analyzed by the first trapping device to enter the detection device from a sample detection port of the automatic alternating sample injection device for detection;
5) Purge-trap state of the second trap: in the resolving process of the first trapping device, a purging airflow control valve is opened, a drying airflow control valve is closed, and purging gas enters a trapping pipe in the second trapping device from a purging gas inlet of the automatic alternating sample injection device for purging and trapping;
6) Dry state of the second trapping device: after the second trapping device finishes purging and trapping, closing a purging airflow control valve, opening a drying airflow control valve, and enabling the drying gas to enter the second trapping device from a drying gas inlet of the automatic alternating sample injection device for drying;
7) Analysis state of the second trapping device: after the second trapping device is dried, the system control circuit performs valve switching, so that carrier gas enters the second trapping device from a carrier gas inlet to drive a sample in the second trapping device to enter a subsequent detection device;
8) Repeating the steps 2) to 7) to enable the sample to alternately enter the first trapping device and the second trapping device for purging trapping and analysis, and then enter the detection device.
Due to the adoption of the technical scheme, the invention has the following advantages: 1. according to the invention, the two sample inlets are arranged in the automatic alternating sample injection device, and two sample channels which are not mutually interfered can be formed by switching the ports of the electromagnetic valve, so that the automatic alternating sample injection device can be used for purging, trapping or sample injection respectively, the sample purging, trapping, thermal analysis and sample injection time of the sample is effectively shortened, and the requirement of a customer on mass sample measurement is met. 2. The automatic alternating sample injection device is connected by adopting the conventional electromagnetic valve and the three-way valve, and the heating module and the cooling module adopted by the trapping device are conventional equipment, so that the running cost is effectively reduced, and meanwhile, the double barriers of foreign import instrument price and technical monopoly are broken. Therefore, the invention can be widely applied to the field of analysis of samples.
Drawings
FIG. 1 is a schematic diagram of the structure of the present invention;
FIG. 2 is a schematic diagram of an automatic alternating sample injection device according to the present invention;
FIG. 3 is a schematic view of the present invention in an instrument ready state and the first trapping device entering a purge-trapping state;
FIG. 4 is a schematic view of a first trapping device of the present invention entering a dry state;
fig. 5 is a schematic view showing the first trapping device of the present invention entering an analysis state.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings and examples. It is to be understood, however, that the drawings are designed solely for the purposes of providing a better understanding of the invention and are not to be construed as limiting the invention. In the description of the present invention, it should be understood that the terms "first," "second," and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
As shown in fig. 1, the present invention provides an automatic sample injection device, which includes an automatic alternating sample injection device 1, and first and second trapping devices 2 and 3. The purge gas inlet, the dry gas inlet and the carrier gas inlet (i.e. the port b, the port d and the port a in the figure) of the automatic alternating sample injection device 1 are respectively connected with a purge gas source, a dry gas source and a carrier gas source, two pairs of sample outlets of the automatic alternating sample injection device 1 are respectively connected with the first trapping device 2 and the second trapping device 3, and a sample detection port (i.e. the port c in the figure) of the automatic alternating sample injection device 1 is connected with a detection device, wherein the detection device comprises a gas separation chromatographic column 4 (GC), a thermal cracking tube 5 and a detector 6. Wherein, the automatic alternating sample injection device 1 and the first and second trapping devices 2 and 3 are controlled by a system control circuit.
As shown in fig. 2, the automatic alternating sample injection device 1 comprises first to fourth electromagnetic valves V1 to V4 and first to fourth three-way valves T1 to T4, and COM ports of the first electromagnetic valve V1 and the second electromagnetic valve V2 are used as a first pair of sample outlets of the automatic alternating sample injection device 1 and are respectively connected with two ends of the second trapping device 3; the COM ports of the third electromagnetic valve V3 and the fourth electromagnetic valve V4 are used as second pairs of sample outlets of the automatic alternating sample injection device 1 and are respectively connected with two ends of the first trapping device 2; the normally open end (NO end) of the first electromagnetic valve V1 and the normally closed end (NC end) of the fourth electromagnetic valve V4 are connected through a first three-way valve T1, and the other interface of the first three-way valve T1 is used as a carrier gas inlet (namely an a port) to be connected with a carrier gas source; the normally closed end (NC end) of the first electromagnetic valve V1 and the normally open end (NO end) of the fourth electromagnetic valve V4 are connected through a second three-way valve T2, and the other interface of the second three-way valve T2 is used as a dry gas inlet (namely, d port) of the automatic alternating sample injection device 1; the normally open end (NO end) of the second electromagnetic valve V2 and the normally closed end (NC end) of the third electromagnetic valve V3 are connected through a third three-way valve T3, and the other interface of the third three-way valve T3 is used as a sample detection port (namely, a c port) of the automatic alternating sample injection device 1; the normally closed end (NC end) of the second electromagnetic valve V2 is connected with the normally open end (NO end) of the third electromagnetic valve V3 through a fourth three-way valve T4, and the other interface of the fourth three-way valve T4 is used as a purge gas inlet (namely, a port b). Each electromagnetic valve V1-V4 is connected with a system control circuit and is controlled by the system control circuit.
The first and second trapping devices 2,3 are identical in structure, and the first trapping device 2 is described as an example of the present invention, and the trapping device includes a trapping pipe 21 (31), a heating module 22 (32) connected to the trapping pipe 21 (31), and a cooling module 22 (33). Wherein the heating module 22 (32) and the cooling module 23 (33) are connected with and controlled by a system control circuit.
The purge gas inlet and the dry gas inlet of the automatic alternating sample injection device 1 are respectively connected with a purge gas source and a dry gas source through a purge gas connecting component 7 and a dry gas connecting component 8. The purge gas connection assembly 7 comprises a purge gas flow meter 71, a purge gas flow control valve 72 and a sample injection needle 73. One side of the bottom of the purge gas flowmeter 71 is connected with a purge gas source outlet, a purge gas flow control valve 72 is arranged on a pipeline between the purge gas flowmeter 71 and the purge gas source, the other side of the upper part of the purge gas flowmeter 71 is connected with a lateral interface of a sample injection needle 73, the interface above the sample injection needle 73 is connected with a purge gas inlet (b port) of the automatic alternating sample injection device 1, and a needle below the sample injection needle 73 is inserted into a sample bottle. The dry gas connecting component 8 comprises a dry gas flow meter 81, a dry gas flow control valve 82 and a valve 83, the bottom of the dry gas flow meter 81 is connected with a dry gas source outlet, the upper part of the dry gas flow meter 81 is connected with a carrier gas inlet of the automatic alternating sample injection device 1, the dry gas flow control valve 82 is arranged on a pipeline between the dry gas flow meter 81 and the dry gas source, and the valve 83 is arranged on a pipeline between the dry gas flow meter and a dry gas inlet (d port) of the automatic alternating sample injection device.
The carrier gas inlet of the automatic alternating sample injection device 1 is connected with the carrier gas source through a carrier gas connecting assembly 9, the carrier gas connecting assembly 9 comprises a carrier gas flowmeter 91 and a carrier gas flow control valve 92, the bottom of the carrier gas flowmeter 91 is connected with the carrier gas source outlet, the upper part of the carrier gas flowmeter is communicated with the carrier gas inlet (a port) of the automatic alternating sample injection device 1, and the carrier gas flow control valve 92 is arranged on a pipeline between the carrier gas flowmeter 91 and the carrier gas source.
As a preferred embodiment, the automatic alternating sample injection device 1 is connected with the first trapping device 2, the second trapping device 3, the purge gas source, the drying gas source and the carrier gas source by adopting 1/8 Teflon pipelines.
As a preferred embodiment, the heating module in the two trapping devices is a wound resistive heating module.
As a preferred embodiment, the cooling module in the two trapping devices employs a fan cooling module.
As shown in fig. 3 to 5, based on the automatic sample injection device, the invention further provides an automatic sample injection method, which comprises the following steps:
1) Instrument ready state: the purge gas flow control valve 72 and the dry gas flow control valve 82 are closed, and the carrier gas flow control valve 92 is opened, and simultaneously, the collection pipes in the two collection devices 2 and 3 do not work, and the carrier gas enters the detection device from the carrier gas inlet of the automatic alternating sample injection device 1 through the collection pipe of the second collection device 3.
At this time, the tenax collecting pipes in the two collecting devices are in a non-working state, the purge air flow control valve 72 and the dry air flow control valve 82 are closed, the carrier air flow control valve 92 is opened, the carrier air enters the NO end of the electromagnetic valve V1 from the carrier air inlet and flows out from the COM end of the electromagnetic valve V1, passes through the tenax collecting pipe 31 in the second collecting device 3, enters the COM end of the electromagnetic valve V2, flows out from the NO end of the electromagnetic valve V2, and enters the gas separation chromatographic column 4, the thermal cracking tube 5 and the detector 6 through the detection sample port c.
2) Purge-trap state of the first trap 2: the carrier gas flow control valve 92 is kept unchanged, the purge gas flow control valve 72 is opened, and the trap pipe 21 in the first trapping device 2 works to trap the sample entering from the purge gas inlet of the automatic alternating sample feeding device 1.
As shown in fig. 3, the present invention is described by taking the first trapping device 2 as an example, which is first put into operation. When purging and trapping, the carrier gas still runs according to the ready state of the instrument; the purge gas flow control valve 72 is opened, the purge gas enters the automatic alternating sample injection device 1 through the sample injection needle and the sample bottle, the purge gas enters the NO end of the electromagnetic valve V3, flows out of the COM end of the electromagnetic valve V3, catches the sample through the tenax collecting pipe 21 in the first collecting device 2, enters the COM end of the electromagnetic valve V4, flows out of the normal open end of the electromagnetic valve V4, and is discharged to the valve 83 through the dry gas inlet and discharged into the waste collecting device.
3) Dry state of the first trapping device 2: after the purge and the collection are completed, the carrier gas flow control valve 92 is kept unchanged, the purge gas flow control valve 72 is closed, the dry gas flow control valve 82 is opened, and the dry gas enters the sample collected by the first collection device 2 from the dry gas inlet of the automatic alternating sample injection device 1 to be dried.
As shown in fig. 4, the carrier gas is still operating in the instrument ready state during drying; the dry gas flow control valve 82 is opened, dry gas enters the automatic alternating sample injection device 1 from a dry gas inlet, dry gas flows in from the normally open end of the electromagnetic valve V4, enters the first trapping device 2 through the COM end of the electromagnetic valve V4, flows out from the upper end of the first trapping device 2 and then enters the COM end of the electromagnetic valve V3, then flows out from the normally open end of the electromagnetic valve V3, is discharged to the sample injection needle 73 in the purge gas connecting assembly 7 through a purge gas inlet, and is discharged from the middle part of the sample injection needle 73.
4) Analysis state of the first capturing device 2: after the drying is finished, all electromagnetic valves in the automatic switching control device are switched by a system control circuit, meanwhile, the purging airflow control valve 72 and the drying airflow control valve 82 are closed, the carrier gas flow control valve 92 is opened, and the carrier gas drives the sample analyzed by the first trapping device 2 to enter the detection device from the sample detection port of the automatic alternating sample injection device for detection.
As shown in fig. 5, when the first trapping device is in analysis, the 4 solenoid valves V1 to V4 are controlled by the circuit system to switch the valves so that the NO end of each solenoid valve is closed and the NC end is opened, and simultaneously the purge gas flow rate control valve 72 and the dry gas flow rate control valve 82 are closed, and the carrier gas flow rate control valve 92 is opened. The specific working process is as follows: carrier gas flows in from the NC end of the electromagnetic valve V4, flows out from the COM end of the electromagnetic valve V4, enters from the lower end of a tenax collecting pipe in the first collecting device, and meanwhile, the heating module works, and analyzed gas enters the COM end of the electromagnetic valve V3, flows out from the NC end of the electromagnetic valve V3, and enters the gas separation chromatographic column, the thermal cracking pipe and the detector through the sample detection port c.
5) Purge-trap state of the second trap 3: in the resolving process of the first trapping device 2, the purge gas flow control valve 72 is opened, the dry gas flow control valve 82 is closed, and purge gas enters the trapping pipe 31 in the second trapping device 3 from the purge gas inlet of the automatic alternating sample injection device 1 for purge and trapping.
During the resolving process of the first trapping device 2, the tenax trapping pipe 31 in the second trapping device 3 may be in a ready state or a purge trapping or drying state (dual-channel alternate sampling effect). When in a purging and trapping state, the purging air flow control valve 72 is opened, purging air enters the automatic alternating sample injection device 1 through a purging air inlet, enters the NC end of the electromagnetic valve V2, flows out from the COM end of the electromagnetic valve V2, enters the COM end of the electromagnetic valve V1 after passing through the tenax trapping pipe 31 in the second trapping device 3, flows out from the NC end of the electromagnetic valve V1, and is discharged to the valve 83 through a drying air inlet and then discharged into the waste collecting device.
6) Dry state of the second trapping device 3: after the second trapping device 3 finishes purging and trapping, the purging airflow control valve 72 is closed, the drying airflow control valve 82 is opened, and the drying gas enters the second trapping device from the drying gas inlet of the automatic alternating sample feeding device for drying.
When in a dry state, the dry air flow control valve 82 is opened, dry air enters the automatic alternating sample injection device 1 from the dry air inlet, enters the normally closed end of the electromagnetic valve V1, enters the second trapping device 3 through the COM end of the electromagnetic valve V1, enters the COM end of the electromagnetic valve V2 after flowing out from the upper end of the second trapping device 3, then flows out from the normally closed end of the electromagnetic valve V2, is discharged to the sample injection needle 73 in the purge gas connecting assembly 7 through the purge gas inlet, and is discharged from the middle part of the sample injection needle 73.
7) Analysis state of the second capturing device 3: after the second trapping device 3 is dried, the system control circuit performs valve switching, so that the carrier gas enters the second trapping device 3 from the carrier gas inlet and drives the sample in the second trapping device 3 to enter the subsequent detection device.
8) Repeating the steps 2) to 7) to enable the sample to alternately enter the first trapping device 2 and the second trapping device 3 for purging trapping and analysis, and then enter the detection device. The dual-channel alternate sample injection effect is achieved, the waiting time for purging and trapping is greatly saved, and the working efficiency of the instrument is improved.
The foregoing embodiments are only for illustrating the present invention, wherein the structures, connection modes, manufacturing processes, etc. of the components may be changed, and all equivalent changes and modifications performed on the basis of the technical solutions of the present invention should not be excluded from the protection scope of the present invention.
Claims (9)
1. An automatic sampling device, its characterized in that: the device comprises an automatic alternating sample injection device, a first trapping device and a second trapping device; the purge gas inlet, the dry gas inlet and the carrier gas inlet of the automatic alternating sample injection device are respectively connected with a purge gas source, a dry gas source and a carrier gas source, two pairs of sample outlets of the automatic alternating sample injection device are respectively connected with the first trapping device and the second trapping device, and a sample detection port of the automatic alternating sample injection device is connected with the detection device; the automatic alternating sample injection device, the first trapping device and the second trapping device are controlled by a system control circuit;
The automatic alternating sample injection device comprises first to fourth electromagnetic valves and first to fourth three-way valves;
the COM ports of the first electromagnetic valve and the second electromagnetic valve are used as a first pair of sample outlets of the automatic alternating sample injection device and are respectively connected with two ends of the second trapping device;
The COM ports of the third electromagnetic valve and the fourth electromagnetic valve are used as second pairs of sample outlets of the automatic alternating sample injection device and are respectively connected with two ends of the first trapping device;
The normally-open end of the first electromagnetic valve is connected with the normally-closed end of the fourth electromagnetic valve through the first three-way valve, and the other interface of the first three-way valve is used as a carrier gas inlet to be connected with a carrier gas source;
The normally closed end of the first electromagnetic valve and the normally open end of the fourth electromagnetic valve are connected through the second three-way valve, and the other interface of the second three-way valve is used as a dry gas inlet of the automatic alternating sample injection device;
The normal open end of the second electromagnetic valve is connected with the normal closed end of the third electromagnetic valve through the third three-way valve, and the other interface of the third three-way valve is used as a sample detection port of the automatic alternating sample injection device;
The normally closed end of the second electromagnetic valve is connected with the normally open end of the third electromagnetic valve through the fourth three-way valve, and the other interface of the fourth three-way valve is used as a purge gas inlet of the automatic alternating sample injection device;
Each electromagnetic valve is connected with a system control circuit and is controlled by the system control circuit.
2. The autosampler device of claim 1, wherein: the first trapping device and the second trapping device have the same structure, and each of the first trapping device and the second trapping device comprises a trapping pipe, a heating module and a cooling module which are connected with the trapping pipe; the heating module and the cooling module are both connected with the system control circuit and controlled by the system control circuit.
3. An autosampler as claimed in claim 2, wherein: the heating module adopts a winding resistance type heating module, and the cooling module adopts a fan cooling module.
4. The autosampler device of claim 1, wherein: the automatic alternating sample injection device comprises a blowing gas inlet, a drying gas inlet, a blowing gas connecting assembly, a drying gas connecting assembly, a carrier gas inlet, a carrier gas connecting assembly and a carrier gas source.
5. The autosampler of claim 4, wherein: the purge gas connecting component comprises a purge gas flowmeter, a purge gas flow control valve and a sample injection needle; one side of the bottom of the purging airflow meter is connected with a purging gas source outlet, a purging airflow control valve is arranged on a pipeline between the purging airflow meter and the purging gas source, the upper part of the purging airflow meter is connected with a lateral interface of a sample injection needle, the interface above the sample injection needle is connected with a purging gas inlet of the automatic alternating sample injection device, and a needle below the sample injection needle is inserted into a sample bottle.
6. The autosampler of claim 4, wherein: the drying gas connecting assembly comprises a drying gas flowmeter, a drying gas flow control valve and a valve, wherein the bottom of the drying gas flowmeter is connected with a drying gas source outlet, the upper part of the drying gas flowmeter is connected with a carrier gas inlet of the automatic alternating sample injection device, the drying gas flow control valve is arranged on a pipeline between the drying gas flowmeter and the drying gas source, and the valve is arranged on a pipeline between the drying gas flowmeter and the drying gas inlet of the automatic alternating sample injection device.
7. The autosampler of claim 4, wherein: the carrier gas connecting assembly comprises a carrier gas flowmeter and a carrier gas flow control valve, the bottom of the carrier gas flowmeter is connected with a carrier gas source outlet, the upper part of the carrier gas flowmeter is communicated with a carrier gas inlet of the automatic alternating sample injection device, and the carrier gas flow control valve is arranged on a pipeline between the carrier gas flowmeter and the carrier gas source.
8. The autosampler device of claim 1, wherein: the automatic alternating sample injection device is connected with the first trapping device, the second trapping device, the purging gas source, the drying gas source and the carrier gas source through 1/8 Teflon pipelines.
9. An autosampler method using the device according to any one of claims 1 to 8, comprising the steps of:
1) Instrument ready state: closing a purging air flow control valve and a drying air flow control valve, opening a carrier gas flow control valve, enabling the collecting pipes in the two collecting devices to be inoperative, and enabling carrier gas to enter the detecting device through the carrier gas inlet of the automatic alternating sample feeding device after entering the collecting pipe of the second collecting device;
2) Purge-trap state of the first trap: keeping the carrier gas flow control valve unchanged, opening the purge gas flow control valve, and simultaneously, working a trapping pipe in the first trapping device to trap a sample entering from a purge gas inlet of the automatic alternating sample injection device;
3) Dry state of the first trapping device: after purging and trapping are completed, keeping the carrier gas flow control valve unchanged, closing the purging air flow control valve, and opening the drying air flow control valve, wherein the drying air enters a drying air inlet of the automatic alternating sample injection device to dry the sample trapped by the first trapping device;
4) Analysis state of the first trapping device: after the drying is finished, valve switching is carried out on all electromagnetic valves in the automatic switching control device through a system control circuit, meanwhile, a purging airflow control valve and a drying airflow control valve are closed, a carrier gas flow control valve is opened, and the carrier gas drives a sample analyzed by the first trapping device to enter the detection device from a sample detection port of the automatic alternating sample injection device for detection;
5) Purge-trap state of the second trap: in the resolving process of the first trapping device, a purging airflow control valve is opened, a drying airflow control valve is closed, and purging gas enters a trapping pipe in the second trapping device from a purging gas inlet of the automatic alternating sample injection device for purging and trapping;
6) Dry state of the second trapping device: after the second trapping device finishes purging and trapping, closing a purging airflow control valve, opening a drying airflow control valve, and enabling the drying gas to enter the second trapping device from a drying gas inlet of the automatic alternating sample injection device for drying;
7) Analysis state of the second trapping device: after the second trapping device is dried, the system control circuit performs valve switching, so that carrier gas enters the second trapping device from a carrier gas inlet to drive a sample in the second trapping device to enter a subsequent detection device;
8) Repeating the steps 2) to 7) to enable the sample to alternately enter the first trapping device and the second trapping device for purging trapping and analysis, and then enter the detection device.
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| CN112881702B (en) * | 2019-11-30 | 2022-11-18 | 深圳市帝迈生物技术有限公司 | Blood detection device and method and computer storage medium |
| CN114280187A (en) * | 2021-12-24 | 2022-04-05 | 生态环境部南京环境科学研究所 | Method and equipment for detecting and analyzing benzene series in underground water of polluted site |
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