CN106248469A - A kind of continuous micro-extraction device of drop being automatically replenished collection drop and extracting process - Google Patents
A kind of continuous micro-extraction device of drop being automatically replenished collection drop and extracting process Download PDFInfo
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- CN106248469A CN106248469A CN201610929121.3A CN201610929121A CN106248469A CN 106248469 A CN106248469 A CN 106248469A CN 201610929121 A CN201610929121 A CN 201610929121A CN 106248469 A CN106248469 A CN 106248469A
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- 238000004853 microextraction Methods 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 31
- 230000008569 process Effects 0.000 title claims abstract description 22
- 239000000284 extract Substances 0.000 claims abstract description 68
- 238000000605 extraction Methods 0.000 claims abstract description 67
- 239000007788 liquid Substances 0.000 claims abstract description 56
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 26
- 239000000523 sample Substances 0.000 claims description 37
- 239000000835 fiber Substances 0.000 claims description 20
- 239000002699 waste material Substances 0.000 claims description 17
- 239000013307 optical fiber Substances 0.000 claims description 12
- 239000012468 concentrated sample Substances 0.000 claims description 11
- 238000004458 analytical method Methods 0.000 claims description 10
- 238000007789 sealing Methods 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 7
- 230000009977 dual effect Effects 0.000 claims description 6
- 230000008676 import Effects 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 230000037361 pathway Effects 0.000 claims description 6
- 238000012360 testing method Methods 0.000 claims description 6
- 230000015572 biosynthetic process Effects 0.000 claims description 5
- 238000010926 purge Methods 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 239000013589 supplement Substances 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 238000005260 corrosion Methods 0.000 claims description 3
- 230000007797 corrosion Effects 0.000 claims description 3
- 230000011664 signaling Effects 0.000 claims description 3
- 206010010904 Convulsion Diseases 0.000 claims description 2
- 230000008859 change Effects 0.000 claims description 2
- 230000036461 convulsion Effects 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 claims 1
- 238000007689 inspection Methods 0.000 claims 1
- 238000002360 preparation method Methods 0.000 claims 1
- 239000007789 gas Substances 0.000 description 73
- 239000003570 air Substances 0.000 description 14
- 239000012071 phase Substances 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 238000001334 liquid-phase micro-extraction Methods 0.000 description 3
- 238000012544 monitoring process Methods 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 208000035126 Facies Diseases 0.000 description 1
- 239000012080 ambient air Substances 0.000 description 1
- 239000012491 analyte Substances 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 231100000693 bioaccumulation Toxicity 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000005251 capillar electrophoresis Methods 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
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- 238000000746 purification Methods 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000002516 single-drop micro-extraction Methods 0.000 description 1
- 230000009469 supplementation Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4044—Concentrating samples by chemical techniques; Digestion; Chemical decomposition
Abstract
The invention belongs to micro-extraction device technical field, be specifically related to a kind of continuous micro-extraction device of drop and extracting process being automatically replenished and collecting drop.It is an object of the invention to provide a kind of easy and simple to handle, rate of extraction is fast and automaticity is high is automatically replenished the continuous micro-extraction device of drop and the extracting process collecting drop.The present invention is automatically replenished the continuous micro-extraction device of drop collecting drop, including drop replenishment control part, drop is collected and is controlled part and gas flow-rate control section, reagent bottle is communicated with drop replenishment control part by first liquid pipeline, extract is delivered in extracting head to realize the control to extract by drop replenishment control part again by second liquid pipeline, described drop is collected and is controlled partly to pass to mutually with extracting head take the drop of extracting head lower end away collection by collecting pipe, it is provided with gas access in the bottom in extraction chamber, gas flow controls part and passes to take away the gas of extraction intracavity by the top of gas piping with extraction chamber mutually.
Description
Technical field
The invention belongs to micro-extraction device technical field, be specifically related to a kind of be automatically replenished collect drop drop the most micro-
Extraction equipment and extracting process.
Technical background
Liquid-phase micro extraction technique is to propose in the mid-90 in 20th century, and a kind of novel sample developed rapidly
Pretreatment technology.Liquid-phase micro extraction technique integrates sampling, separation, purification, concentration, sample introduction, and adapts to complex dielectrics, trace
Amount composition, the analysis of special nature composition；Simple to operate, quick, it is not necessary to special instruments and equipment；Extraction mode is many, available
Organic solvent kind is many and consumption is the most several to tens microlitres, provides the biggest space for optimizing the condition of liquid-phase micro-extraction.
In the today building resource-efficient and environment friendly society, use the sample that environmental protection, consumption of organic solvent are little and inexpensive
Product pre-treating method has important practical significance.
Single micro-extraction SDME technology is a kind of Sample Pretreatment Technique novel, eco-friendly, and its collection extracts, is enriched in
Integrally, have low cost, device is simple, easily operated, consumption of organic solvent is few and bioaccumulation efficiency high.Single micro-extraction
Take the GC microsyringe needle tip being an extractant is suspended from routine, be then dipped in sample solution or be suspended from sample
Headroom, makes analyte be transferred to organic extractant phase solvent from aqueous phase, through certain time, organic microdroplet is drawn back syringe also
It is transferred to GC or other analysis systems are analyzed.But micro-extraction technique continuous for drop rarely has correlational study and document report
Road.
Summary of the invention
It is an object of the invention to provide a kind of easy and simple to handle, rate of extraction is fast and automaticity is high is automatically replenished collection
The continuous micro-extraction device of drop of drop and extracting process.
The technical scheme that the present invention takes for achieving the above object is:
A kind of continuous micro-extraction device of drop being automatically replenished collection drop, including reagent bottle, at reagent bottle built with extraction
Take liquid, extraction chamber and extracting head, the most also include that drop replenishment control part, drop are collected and control part and gas flow-control
Part, extracting head is arranged on extraction intracavity, and reagent bottle passes to try with drop replenishment control part by first liquid pipeline mutually
Extract in agent bottle is delivered in drop replenishment control part, and drop replenishment control part again will extraction by second liquid pipeline
Taking liquid and be delivered to the interior control with realization to extract of extracting head, described drop is collected and is controlled partly to pass through collecting pipe and extraction
Head passes to take the drop of extracting head lower end away collection mutually, is provided with gas access, gas flow control portion in the bottom in extraction chamber
Divide the gas passing to take away extraction intracavity by the top of gas piping and extraction chamber mutually.
Further, drop replenishment control part of the present invention include drop replenishment control device, the first syringe,
One motor, two piston sensors, first piston, fiber amplifier and reflection-type optical fiber probe, the first syringe passes through first
Liquid line communicates with reagent bottle, the first motor by the first push rod of the first threaded rod and the first syringe bottom be connected with
Drive the first piston at the first push rod top that the extract in the first syringe realizes trace control by the first push rod, two
Piston sensor is separately positioned on first piston and can arrive at minimum capacity position and the maximum capacity position of the first syringe,
Two piston sensors are all connected with drop replenishment control device and feed back to drop with the position signalling by the first piston of collection
Replenishment control device, drop replenishment control device is also connected the rotation controlling the first motor, described reflection type optical with the first motor
Fine probe is arranged on the bottom in extraction chamber and through extraction chamber in the face of drop, reflection-type optical fiber are popped one's head in by launching fiber and reception
Optical fiber is connected with fiber amplifier, and fiber amplifier is connected with drop replenishment control device, and fibre-optical probe sends light and receives
The reflection light of droplet formation, light intensity signal sends to described drop replenishment control device after fiber amplifier processes.
Drop of the present invention is collected control part and is included drop collection controller, the second syringe, the second motor, cuts
Changing valve, collecting pipe, cleaning pipe, sewer pipe, waste liquid bottle and probe tube, described second motor is by the second threaded rod and the second injection
Second push rod at device rear portion is connected the second piston to be driven the second push rod top by the second push rod in the second syringe
Extract realize trace control, at least provided with a switching channel and four fixing passages on described switching valve, i.e. first is solid
Routing, second fix passage, the 3rd fix passage, the 4th fix passage, the fixing end of switching channel and the second syringe phase
Logical, the movable end of switching channel can be fixed passage respectively, second fix passage, the 3rd fixes passage, the 4th fixing logical with first
Road communicates, and first fixes passage is connected with one end of collecting pipe, and the other end of collecting pipe contacts with the lower end of extracting head use
In collecting drop and stoping drop to be back in extracting head, second fixes passage is connected with the one end cleaning pipe, cleans pipe
The other end and the extract in reagent bottle are common to clean the second syringe mutually, and the 3rd fixes passage is connected with one end of sewer pipe
Connecing, the other end of sewer pipe is connected with waste liquid bottle and cleans waste liquid that the second syringe produces in waste liquid bottle for discharging, the
Four fix passage is connected with one end of probe tube, and the other end of probe tube is connected with concentrated sample introduction bottle or detecting instrument use
In the drop collected of transmission to concentrated sample introduction bottle or detecting instrument.
Gas flow control part of the present invention includes gas flow controller, gas flow sensor, miniature takes out
Blower fan, miniature air exhauster and gas flow sensor be all disposed within gas exit line, gas flow sensor and gas stream
Amount controller is connected and the gas flow signals of collection sends to gas flow controller, and gas flow controller is taken out with miniature
Blower fan is connected and controls gas according to certain flow from entrance entrance extraction chamber purging with the rotation by the miniature air exhauster of control
Discharging from gas exit line after drop, miniature air exhauster is communicated by the top of gas piping with extraction chamber.
The entrance in extraction chamber of the present invention can connect a road as required and examine for instrument to multichannel gas to be measured
Survey.
The top of extracting head of the present invention is provided with sealing dottle pin.
The bottom of extracting head of the present invention is provided with attaching device.
Attaching device of the present invention is helical form.
Collecting pipe of the present invention is the circular bell-mouth structure of air launched near one end of extracting head.
First syringe top of the present invention has dual pathways plug, and dual pathways plug connects only import but no export respectively
Reverse valve and the forward valve of only export but no import；Reagent bottle and the first syringe are connected by described reverse valve by first liquid pipeline,
Extract can only enter the first syringe through described reverse valve and cannot discharge；Described forward valve is by through sealing the of dottle pin
First syringe is connected by two liquid lines with extracting head, and extract can only be discharged the first syringe through described forward valve and cannot
Enter.
Extracting head of the present invention and extraction chamber is quartz glass material or corrosion resistant material is made；Described extraction
Chamber upper end open has interior ground, agrees with the outer grinding port of described extracting head upper end；The upper end of described extracting head has fixed bit to use
Sealing dottle pin with chemical stability flexible with fixture, the lower end of described extracting head is fixedly connected the upper of attaching device
Portion, the bottom of attaching device extends down and do not have external stability to connect, and the extract in described extracting head relies on surface tension
It is attached to attaching device bottom and hangs formation drop at its end.
A kind of extracting process being automatically replenished the continuous micro-extraction device of drop collecting drop, comprises the following steps:
A determines that extract forms, and uses one or more solvents to prepare extract, joins after filtering in reagent bottle；
B starts drop collection controller, and the switching channel of control switching valve is communicated to second and fixes passage, controls the second electricity
Machine pulls the second syringe extraction extract to be communicated to the 3rd and fix passage to heap(ed) capacity, control switching channel, control second
Motor pushing the second syringe discharges whole extracts in waste liquid bottle, repeated multiple times to clean the second syringe；
C starts gas flow controller, determines the gas flow entering extraction chamber, controls gas stream by miniature air exhauster
Amount, monitors gas flow by gas flow sensor；
D starts drop replenishment control device, control the first motor pull the first syringe extraction extract to heap(ed) capacity, with
Rear control the first motor promotes at a slow speed the first syringe to discharge extract in extracting head, makes in extracting head and attaching device bottom
It is full of the drop that hanging also occurs in extract, stops until drop reaches to control the first motor during full or trystate；
When e drop replenishment control device reaches full or trystate by fiber amplifier and fibre-optical probe record drop
Intensity of reflected light, control the marginal value of the first motor start and stop in this, as drop replenishment control device；
Gas to be measured is accessed the entrance in extraction chamber and starts timing by f, gas to be measured carries out drop from now on even
Continuous micro-extraction；
The continuous of drop is purged by g along with gas, and extract constantly volatilizees and causes droplet size to diminish, and fibre-optical probe is monitored
The intensity of reflected light arrived is less than marginal value, then drop replenishment control device starts the first motor and promotes at a slow speed the first syringe to drop
Supplement in time；
H is when the intensity of reflected light that drop is supplemented, fibre-optical probe monitors is at or above marginal value, and drop is mended
Fill controller and stop the first motor the most immediately；
I utilizes drop replenishment control device automatically to repeat g step and the process of h step, until it reaches the time of testing requirement
Or gas detecting to be measured is complete；
J stops drop replenishment control device, and the switching channel utilizing drop collection controller to control switching valve is communicated to first
Fixing passage, controls the second motor and pulls the second syringe to extract the liquid to be measured in attaching device bottom and drop completely, controls
Switching channel is communicated to the 4th and fixes passage, controls second motor pushing the second syringe and is completely exhausted out liquid to be measured to concentrated sample introduction
In Ping, machine analysis detection in wait；
K repeats b and walks process, cleans the second syringe；
L drop replenishment control device waits the beginning of next drop continuous micro-extraction process；
M is when the first piston of the first syringe arrives minimum capacity position, and drop replenishment control device then controls the first electricity
Machine pulls the first syringe extraction extract to heap(ed) capacity.
The continuous micro-extraction of drop of the present invention is to carry the continuously gas of flowing of component to be measured constantly to purge and persistently wave
Send out and realized between flowing gas and volume continually varying drop by the drop of continuous supplementation, component to be measured the extraction of dynamic equilibrium
Take process, can be used for the extraction of volatile component, enrichment in one or more gases；Droplet size during the continuous micro-extraction of drop
Within the specific limits the moment change, excursion depend mainly on the size of the drop replenishment control device control energy to droplet size
Power and the flow of gas to be measured；The purging continuously of gas causes extract persistently to volatilize, this to be measured group be extracted into drop
Dividing and have enrichment method effect, the flow of gas should not excessive be avoided making drop drop.Drop replenishment control device of the present invention
Power is provided with described drop collection controller the respectively first motor, the second motor and its rotating speed or amount of spin are had essence
Really control ability；Described drop replenishment control device and described drop collection controller have the information processing function, by editor's journey
Sequence and setup control parameter realize being automatically replenished drop and automatically collecting.
The method have the advantages that
1, device achieves being automatically replenished and automatically collecting of extract drop, provides for the continuous micro-extraction technique of drop
A kind of effective and feasible automaton, the convenient multiple analysis such as with gas chromatography-mass spectrum, liquid chromatography-mass spectrography, capillary electrophoresis
Detecting instrument is combined.
2, device have simplicity, quickly, stable, efficient feature, during micro-extraction to droplet profile the most accurately
Control provides technical guarantee for carrying out qualitative and quantitative detection.
3, device achieves the continuous extraction enrichment of volatile component in one or more mixed gas and automatic sampling
The continuous micro-extraction technique of sample introduction, beneficially drop is at the analysis of thermal analyzer emergent gas, Chemical Manufacture on-line monitoring, surrounding air
The application of the aspects such as quality monitoring automatically.
Accompanying drawing explanation
Fig. 1 is the structural representation of the present invention.
Detailed description of the invention
Embodiment 1
It is automatically replenished the continuous micro-extraction device of drop collecting drop, including reagent bottle 8, at reagent as it is shown in figure 1, a kind of
Bottle 8, built with extract 7, extraction chamber 25 and extracting head 19, the most also includes that drop replenishment control part, drop collect control portion
Dividing and gas flow-rate control section, extraction chamber 25 upper end open has interior ground, and extracting head 19 upper end is provided with outer grinding port, extracting head
In 19 are arranged on extraction chamber 25 and agreed with by interior ground and outer grinding port and there is air seal effect, in the upper end of extracting head 19
Having fixed bit flexible in order to fixture and the sealing dottle pin 21 of chemical stability, the bottom of extracting head 19 is provided with helical form attaching
Device 23, the lower end of extracting head 19 is fixedly connected the top of attaching device 23, and the bottom of attaching device 23 extends down and do not have
Having external stability to connect, the extract 7 in described extracting head 19 relies on surface tension to be attached to attaching device 23 bottom and at it
End hangs and forms drop 24, and reagent bottle 8 is passed to reagent bottle 8 with drop replenishment control part mutually by first liquid pipeline 9
Interior extract 7 is delivered in drop replenishment control part, and drop replenishment control part will be extracted by second liquid pipeline 9a again
Taking liquid 7 and be delivered to the interior control with realization to extract 7 of extracting head 19, described drop is collected and is controlled partly to pass through collecting pipe 36
Pass to take the drop 24 of extracting head 19 lower end away collection with extracting head 19 phase, be provided with air intake 1 in the bottom in extraction chamber 25,
Gas flow controls part and passes to mutually take the air in extraction chamber 25 away by the top of gas piping 26 with extraction chamber 25.
Described drop replenishment control part includes drop replenishment control device the 2, first syringe the 14, first motor 18, two
Individual piston sensor 11, first piston 15, fiber amplifier 3 and reflection-type optical fiber probe 4, the first syringe 14 is by the first liquid
Body pipeline 9 communicates with reagent bottle 8, and the first motor 18 is by the first threaded rod 16 and the first push rod 17 of the first syringe 14 bottom
It is connected to be driven the first piston 15 at the first push rod 17 top to the extract 7 in the first syringe 14 by the first push rod 17
Realizing trace control, two piston sensors 11 are separately positioned on first piston 15 and can arrive the minimum appearance of the first syringe 14
At amount position and maximum capacity position, two piston sensors 11 be all connected with drop replenishment control device 2 with will gather the
The position signalling of one piston 15 feeds back to drop replenishment control device 2, drop replenishment control device 2 be also connected with the first motor 18 with
Controlling the rotation of the first motor 18, have dual pathways plug 13 on the first syringe 14 top, dual pathways plug 13 connects respectively
The reverse valve 10 of only import but no export and the forward valve 12 of only export but no import, described reverse valve 10 passes through first liquid pipeline 9 by reagent bottle 8
Connecting with the first syringe 14, extract 7 can only enter the first syringe 14 through described reverse valve 10 and cannot discharge, described just
To valve 12 by first syringe 14 being connected with extracting head 19 through the second liquid pipeline 9a sealing dottle pin 21, extract 7
Can only discharge the first syringe 14 through described forward valve 12 and cannot be introduced into, described reflection-type optical fiber probe 4 is arranged on extraction chamber
The bottom of 25 and through extraction chamber 25 in the face of drop 24, reflection-type optical fiber probe 4 is by launching fiber 5 and receives optical fiber 6 and light
Fiber amplifier 3 is connected, and fiber amplifier 3 is connected with drop replenishment control device 2, and fibre-optical probe 4 sends light and receives drop
The 24 reflection light formed, light intensity signal sends to described drop replenishment control device 2 after fiber amplifier 3 processes.
Described drop collect control part include drop collection controller the 31, second syringe 14a, the second motor 18a,
Switching valve 32, collecting pipe 36, cleaning pipe 37, sewer pipe 38, waste liquid bottle 40 and probe tube 39, described second motor 18a is by the
The second push rod 17a at two threaded rod 16a and the second syringe 14a rear portion is connected to drive second to push away by the second push rod 17a
The second piston 15a at bar 17a top realizes trace control to the extract 7 in the second syringe 14a, and described switching valve 32 is up to
It is provided with a switching channel 35 and four fixing passages less, i.e. first fixes passage 33a, second fix passage 33b, the 3rd fix
Passage 33c, the 4th fixing passage 33d, fixing end and the second syringe 14a of switching channel 35 communicate, the work of switching channel 35
Moved end can be fixed passage 33a respectively, second fix passage 33b, the 3rd fixes passage 33c, the 4th fixes passage 33d phase with first
Logical, first fixes passage 33a is connected with one end of collecting pipe 36, and the other end of collecting pipe 36 is the circular horn mouth 22 launched
Structure and be arranged on the lower end of extracting head 19 for collecting drop 24 and stoping drop 24 to be back in extracting head 19, second fixes
Passage 33b is connected with the one end cleaning pipe 37, and the other end cleaning pipe 37 is common to clearly with extract 7 phase in reagent bottle 8
Washing the second syringe 14a, the 3rd fixes passage 33c is connected with one end of sewer pipe 38, the other end of sewer pipe 38 and waste liquid
Bottle 40 is connected and cleans waste liquid that the second syringe 14a produces in waste liquid bottle 40 for discharging, and the 4th fixes passage 33d and take
One end of sample pipe 39 is connected, and the other end of probe tube 39 is connected for transmitting receipts with concentrated sample introduction bottle 41 or detecting instrument
Collect to drop 24 to concentrated sample introduction bottle 41 or detecting instrument in.
Described gas flow control part includes gas flow controller 28, gas flow sensor 29, miniature convulsion
Machine 27, miniature air exhauster 27 and gas flow sensor 29 be all disposed within gas exit line 30, gas flow sensor 29
It is connected with gas flow controller 28 and sends the gas flow signals of collection to gas flow controller 28, gas flow
Controller 28 is connected with miniature air exhauster 27 with the rotation control gas by controlling miniature air exhauster 27 according to certain flow
Entering after extraction chamber 25 purges drop 24 from entrance 1 and discharge from gas exit line 30, miniature air exhauster 27 passes through gas piping
26 communicate with the top in extraction chamber 25.
The entrance 1 in the extraction chamber 25 described in the present embodiment can connect a road as required to multichannel gas to be measured, application
In aspects such as the analysis of thermal analyzer emergent gas, Chemical Manufacture on-line monitoring, ambient air quality detections.
Extracting head 19 and extraction chamber 25 described in the present embodiment are made for quartz glass material or corrosion resistant material.
Embodiment 2
A kind of extracting process being automatically replenished the continuous micro-extraction device of drop collecting drop, comprises the following steps:
A determines that extract 7 forms, and uses one or more solvents to prepare extract 7, joins reagent bottle 8 after filtering
In；
B starts drop collection controller 31, and the switching channel 35 of control switching valve 32 is communicated to second and fixes passage 33b,
Controlling the second motor 18a pulls the second syringe 14a to extract extract 7 to heap(ed) capacity, controls switching channel 35 and is communicated to the
Three fix passage 33c, control the second motor 18a and promote the second syringe 14a to discharge in whole extract 7 to waste liquid bottles 40, instead
Multiple repeatedly to clean the second syringe 14a；
C starts gas flow controller 28, determines the gas flow entering extraction chamber 25, is controlled by miniature air exhauster 27
Gas flow, monitors gas flow by gas flow sensor 29；
D starts drop replenishment control device 2, controls the first motor 18 and pulls the first syringe 14 to extract extract 7 to maximum
Capacity, controls the first motor 18 subsequently and promotes at a slow speed the first syringe 14 to discharge in extract 7 to extracting head 19, make extracting head 19
Neutralize attaching device 23 bottom be full of extract 7 and the drop 24 hung occurs, until drop 24 reaches full or test shape
Control the first motor 18 during state to stop；
E drop replenishment control device 2 records drop 24 by fiber amplifier 3 and fibre-optical probe 4 and reaches full or test
Intensity of reflected light during state, controls the marginal value of the first motor 18 start and stop in this, as drop replenishment control device 2；
Gas to be measured is accessed the entrance 1 in extraction chamber 25 and starts timing by f, from now on gas to be measured is carried out drop
Micro-extraction continuously；
The continuous of drop 24 is purged by g along with gas, and extract 7 constantly volatilizees and causes drop 24 volume to diminish, and optical fiber is visited
4 intensities of reflected light monitored are less than marginal value, then drop replenishment control device 2 starts the first motor 18 and promotes at a slow speed the first note
Drop 24 is supplemented by emitter 14 in time；
H when the intensity of reflected light that drop 24 is supplemented, fibre-optical probe 4 monitors at or above marginal value time, liquid
Drip replenishment control device 2 and stop the first motor 18 the most immediately；
I utilizes drop replenishment control device 2 automatically to repeat g step and the process of h step, until it reaches the time of testing requirement
Or gas detecting to be measured is complete；
J stops drop replenishment control device 2, and the switching channel 35 utilizing drop collection controller 31 to control switching valve 32 connects
Fix passage 33a to first, control the second motor 18a and pull the second syringe 14a to extract attaching device 23 bottom and liquid completely
Dripping the liquid to be measured in 24, control switching channel 35 is communicated to the 4th and fixes passage 33d, controls the second motor 18a and promote the second note
Emitter 14a is completely exhausted out liquid to be measured in concentrated sample introduction bottle 41, machine analysis detection in wait；
K repeats b and walks process, cleans the second syringe 14a；
L drop replenishment control device 2 waits the beginning of next drop continuous micro-extraction process；
M is when the first piston 15 of the first syringe 14 arrives minimum capacity position, and drop replenishment control device 2 then controls
One motor 18 pulls the first syringe 14 to extract extract 7 to heap(ed) capacity.
Embodiment 3
The extracting and enriching of volatile component in environmental gas, comprises the following steps:
(1) the gas 30L in indoor environment to be measured, is first collected in collection airbag；
(2), utilize ethanol and isopropanol to prepare 200mL extract according to volume ratio 1:9, take out through 0.22 μm organic facies filter membrane
Vacuum joins in reagent bottle after filtering；
(3), starting drop collection controller, the switching channel controlling switching valve rotates to fixing passage b, controls the second note
Emitter extraction extract, to heap(ed) capacity 100 μ L, controls switching channel and is communicated to fixing passage c, control the second syringe and discharge
All extracts are in waste liquid bottle, and this operation is repeated 3 times to clean the second syringe；
(4), starting gas flow controller, the gas flow being set into extracting chamber is 500mL/min；
(5), start drop replenishment control device, control the first syringe extraction extract at 20mL heap(ed) capacity, subsequently
Control the first syringe and discharge at a slow speed extract, make extracting head and attaching device are full of extract and the drop hung occurs,
Until drop reaches to suspend during full experimental state；
(6) when, drop replenishment control device reaches full experimental state by fiber amplifier and fibre-optical probe record drop
Intensity of reflected light signal value be about 350, control the marginal value of the first syringe start and stop in this, as drop replenishment control device；
(7), the gas to be measured being collected in collection airbag is accessed extraction chamber entrance and carry out the continuous micro-extraction of drop；
(8), when the intensity of reflected light signal value of droplet formation is less than 350, drop replenishment control device controls the first injection
Drop is supplemented by device in time, when intensity of reflected light reaches 350 marginal value the most immediately stop supplement, this operation automatically repeat into
OK, until stopping when gas detecting to be measured is complete；
(9), utilize the switching channel of drop collection controller control switching valve to be communicated to fixing passage a, control the second note
Emitter extracts the liquid to be measured in spiral attaching device bottom and drop completely, controls switching channel and is communicated to fixing passage d, controls
Second syringe is completely exhausted out liquid to be measured in concentrated sample introduction bottle, detects liquid analysis to be measured with gas chromatograph-mass spectrometer (GC-MS)；
(10), repeat the 3rd step operation, clean the second syringe.
Embodiment 4
The continuous micro-extraction of drop of thermal analyzer emergent gas, comprises the following steps:
(1), in thermal analyzer, add testing sample 10mg, set carrier gas flux as 300mL/min, design temperature program
It is 200 DEG C and keeps 20min；
(2), take 200mL ethanol as extract, join in reagent bottle after 0.22 μm membrane filtration；
(3), starting drop collection controller, the switching channel controlling switching valve rotates to fixing passage b, controls the second note
Emitter extraction extract, to heap(ed) capacity 100 μ L, controls switching channel and is communicated to fixing passage c, control the second syringe and discharge
All extracts are in waste liquid bottle, repeat this operation 2 times to clean the second syringe；
(4), start drop replenishment control device, control the first syringe extraction extract at 20mL heap(ed) capacity, subsequently
Control the first syringe and discharge at a slow speed extract, make extracting head and spiral attaching device are full of extract and the liquid hung occurs
Drip, until drop reaches to suspend during full experimental state；
(5) when, drop replenishment control device reaches full experimental state by fiber amplifier and fibre-optical probe record drop
Intensity of reflected light signal value about 300, control the marginal value of the first syringe start and stop in this, as drop replenishment control device；
(6), start thermal analyzer temperature program(me), by the transfer conduit of 150 DEG C of heated for controlling temperatures will escape out gas introduce
Extraction chamber entrance carries out the continuous micro-extraction of drop；
(7), when the intensity of reflected light signal value of droplet formation is less than 300, drop replenishment control device controls the first injection
Drop is supplemented by device in time, when intensity of reflected light reaches 300 marginal value the most immediately stop supplement, this operation automatically repeat into
OK, until stopping at the end of the temperature program(me) of thermal analyzer；
(8), utilize the switching channel of drop collection controller control switching valve to be communicated to fixing passage a, control the second note
Emitter extracts the liquid to be measured in spiral attaching device bottom and drop completely, controls switching channel and is communicated to fixing passage d, controls
Second syringe is completely exhausted out liquid to be measured in concentrated sample introduction bottle, detects liquid analysis to be measured with liquid chromatograph-mass spectrometer.
Claims (12)
1. it is automatically replenished the continuous micro-extraction device of drop collecting drop, including reagent bottle (8), built-in at reagent bottle (8)
There are extract (7), extraction chamber (25) and extracting head (19), it is characterised in that also include that drop replenishment control part, drop are collected
Controlling part and gas flow-rate control section, extracting head (19) is arranged in extraction chamber (25), and reagent bottle (8) passes through first liquid
Pipeline (9) and drop replenishment control part pass to the extract (7) in reagent bottle (8) is delivered to drop replenishment control part mutually
In, it is interior to realize that extract (7) is delivered to extracting head (19) by second liquid pipeline (9a) by drop replenishment control part again
Control to extract (7), described drop is collected and is controlled partly to pass to mutually to extract with extracting head (19) by collecting pipe (36)
The drop (24) taking head (19) lower end takes collection away, is provided with gas access (1) in the bottom of extraction chamber (25), and gas flow controls
Part passes to take the gas in extraction chamber (25) away by the top of gas piping (26) with extraction chamber (25) mutually.
A kind of continuous micro-extraction device of drop being automatically replenished collection drop the most according to claim 1, it is characterised in that
Described drop replenishment control part includes drop replenishment control device (2), the first syringe (14), the first motor (18), two
Piston sensor (11), first piston (15), fiber amplifier (3) and reflection-type optical fiber probe (4), the first syringe (14) leads to
Crossing first liquid pipeline (9) to communicate with reagent bottle (8), the first motor (18) is by the first threaded rod (16) and the first syringe
(14) first push rod (17) of bottom is connected the first piston to be driven the first push rod (17) top by the first push rod (17)
(15) extract (7) in the first syringe (14) realizing trace control, two piston sensors (11) are separately positioned on
One piston (15) can arrive at minimum capacity position and the maximum capacity position of the first syringe (14), two piston sensors
(11) all it is connected with drop replenishment control device (2) and supplements so that the position signalling of first piston (15) gathered is fed back to drop
Controller (2), drop replenishment control device (2) is also connected the rotation controlling the first motor (18), institute with the first motor (18)
State reflection-type optical fiber probe (4) and be arranged on the bottom of extraction chamber (25) and through extraction chamber (25) in the face of drop (24), reflection-type
Fibre-optical probe (4) by launching fiber (5) and receive optical fiber (6) be connected with fiber amplifier (3), fiber amplifier (3) and
Drop replenishment control device (2) is connected, and fibre-optical probe (4) sends light and receives the reflection light that drop (24) is formed, and light intensity is believed
Number send to described drop replenishment control device (2) after fiber amplifier (3) processes.
A kind of continuous micro-extraction device of drop being automatically replenished collection drop the most according to claim 1, it is characterised in that
Described drop is collected control part and is included drop collection controller (31), the second syringe (14a), the second motor (18a), cuts
Change valve (32), collecting pipe (36), clean pipe (37), sewer pipe (38), waste liquid bottle (40) and probe tube (39), described second motor
(18a) it is connected with by second with second push rod (17a) at the second syringe (14a) rear portion by the second threaded rod (16a)
Push rod (17a) drives second piston (15a) at the second push rod (17a) top to the extract (7) in the second syringe (14a) in fact
Existing trace controls, and at least provided with a switching channel (35) and four fixing passages on described switching valve (32), i.e. first fixes
Passage (33a), second fix passage (33b), the 3rd fix passage (33c), the 4th fix passage (33d), switching channel (35)
Fixing end and the second syringe (14a) communicate, the movable end of switching channel (35) can fix with first respectively passage (33a),
Second fix passage (33b), the 3rd fix passage (33c), the 4th fix passage (33d) and communicate, first fix passage (33a) with
One end of collecting pipe (36) is connected, and the other end of collecting pipe (36) contacts for collecting drop with the lower end of extracting head (19)
(24) and in stoping drop (24) to be back to extracting head (19), second fixes passage (33b) is connected with cleaning the one end managing (37)
Connect, clean the pipe other end of (37) and the extract (7) in reagent bottle (8) is common to clean the second syringe (14a) mutually, the 3rd
Fixing passage (33c) is connected with one end of sewer pipe (38), and the other end of sewer pipe (38) is connected with waste liquid bottle (40) use
Cleaning the second syringe (14a) waste liquid that produces in waste liquid bottle (40) in discharging, the 4th fixes passage (33d) and probe tube
(39) one end is connected, and the other end of probe tube (39) is connected for transmitting with concentrated sample introduction bottle (41) or detecting instrument
The drop (24) collected is in concentrated sample introduction bottle (41) or detecting instrument.
A kind of continuous micro-extraction device of drop being automatically replenished collection drop the most according to claim 1, it is characterised in that
Described gas flow controls portion gas flow controller (28), gas flow sensor (29), miniature air exhauster (27), micro-
Type air exhauster (27) and gas flow sensor (29) are all disposed within gas exit line (30), gas flow sensor (29)
It is connected with gas flow controller (28) and the gas flow signals of collection is sent to gas flow controller (28), gas stream
Amount controller (28) be connected with miniature air exhauster (27) with by control miniature air exhauster (27) rotation control gas according to
Certain flow is discharged from gas exit line (30) after entrance (1) enters extraction chamber (25) purging drop (24), miniature convulsion
Machine (27) is communicated by the top of gas piping (26) with extraction chamber (25).
A kind of continuous micro-extraction device of drop being automatically replenished collection drop the most according to claim 1, it is characterised in that
The entrance (1) in described extraction chamber (25) can connect a road as required and detect for instrument to multichannel gas to be measured.
A kind of continuous micro-extraction device of drop being automatically replenished collection drop the most according to claim 1, it is characterised in that
The top of described extracting head (19) is provided with sealing dottle pin (21).
A kind of continuous micro-extraction device of drop being automatically replenished collection drop the most according to claim 1, it is characterised in that
The bottom of described extracting head (19) is provided with attaching device (23) with support and absorption drop (24).
A kind of continuous micro-extraction device of drop being automatically replenished collection drop the most according to claim 7, it is characterised in that
Described attaching device (23) is hollow screw shape.
A kind of continuous micro-extraction device of drop being automatically replenished collection drop the most according to claim 3, it is characterised in that
Described collecting pipe (36) is circular horn mouth (22) structure launched near one end of extracting head (19).
A kind of continuous micro-extraction device of drop being automatically replenished collection drop the most according to claim 2, it is characterised in that
Described the first syringe (14) top has dual pathways plug (13), and dual pathways plug (13) connects the inverse of only import but no export respectively
To the forward valve (12) of valve (10) and only export but no import, described reverse valve (10) by first liquid pipeline (9) by reagent bottle (8) with
First syringe (14) connects, and extract (7) can only enter the first syringe (14) through described reverse valve (10) and cannot discharge,
Described forward valve (12) is by through sealing the second liquid pipeline (9a) of dottle pin (21) by the first syringe (14) and extracting head
(19) connection, extract (7) can only be discharged the first syringe (14) through described forward valve (12) and be cannot be introduced into.
11. a kind of continuous micro-extraction devices of drop being automatically replenished collection drop according to claim 1, it is characterised in that
Described extracting head (19) and extraction chamber (25) are quartz glass material or corrosion resistant material is made, described extraction chamber (25)
Upper end open has interior ground, agrees with the outer grinding port of described extracting head (19) upper end, and the upper end of described extracting head (19) has solid
Positioning flexible in order to fixture and chemical stability sealing dottle pin (21), the lower end of described extracting head (19) is fixedly connected
The top of attaching device (23), the bottom of attaching device (23) extends down and do not have external stability to connect, described extracting head
(19) extract (7) in relies on surface tension be attached to attaching device (23) bottom and hang formation drop at its end
(24)。
In 12. claim 1 to 11, a kind of described in any one is automatically replenished the continuous micro-extraction device of drop collecting drop
Extracting process, it is characterised in that comprise the following steps:
A determines that extract (7) forms, and uses one or more solvents preparation extract (7), joins reagent bottle after filtering
(8) in；
B starts drop collection controller (31), and the switching channel (35) of control switching valve (32) is communicated to second and fixes passage
(33b), control the second motor (18a) and pull the second syringe (14a) extraction extract (7) to heap(ed) capacity, control switching logical
Road (35) is communicated to the 3rd and fixes passage (33c), controls the second motor (18a) and promotes the second syringe (14a) to discharge all extractions
Take liquid (7) in waste liquid bottle (40), repeated multiple times to clean the second syringe (14a)；
C starts gas flow controller (28), determines the gas flow entering extraction chamber (25), is controlled by miniature air exhauster (27)
Gas flow processed, monitors gas flow by gas flow sensor (29)；
D starts drop replenishment control device (2), controls the first motor (18) and pulls the first syringe (14) extraction extract (7) extremely
Heap(ed) capacity, controls the first motor (18) subsequently and promotes at a slow speed the first syringe (14) to discharge extract (7) to extracting head (19)
In, make extracting head (19) neutralize attaching device (23) bottom and be full of extract (7) and the drop (24) hung occurs, until drop
(24) reach during full or trystate, to control the first motor (18) to stop；
E drop replenishment control device (2) by fiber amplifier (3) and fibre-optical probe (4) record drop (24) reach full or
Intensity of reflected light during trystate, controls the marginal value of the first motor (18) start and stop in this, as drop replenishment control device (2)；
Gas to be measured is accessed the entrance (1) of extraction chamber (25) and starts timing by f, from now on gas to be measured is carried out drop
Micro-extraction continuously；
The continuous of drop (24) is purged by g along with gas, and extract (7) constantly volatilization causes drop (24) volume to diminish, optical fiber
Probe (4) intensity of reflected light that monitors is less than marginal value, then drop replenishment control device (2) starts the first motor (18) and pushes away at a slow speed
Drop (24) is supplemented by dynamic first syringe (14) in time；
H when the intensity of reflected light that drop (24) is supplemented, fibre-optical probe (4) monitors at or above marginal value time, liquid
Drip replenishment control device (2) and stop the first motor (18) the most immediately；
I utilizes drop replenishment control device (2) automatically to repeat g step and the process of h step, until it reaches time of testing requirement or
Person's gas detecting to be measured is complete；
J stops drop replenishment control device (2), utilizes drop collection controller (31) to control the switching channel (35) of switching valve (32)
It is communicated to first and fixes passage (33a), control the second motor (18a) and pull the second syringe (14a) to extract attaching device completely
(23) liquid to be measured in bottom and drop (24), controls switching channel (35) and is communicated to the 4th and fixes passage (33d), control second
Motor (18a) promotes the second syringe (14a) to be completely exhausted out liquid to be measured in concentrated sample introduction bottle (41), machine analysis inspection in wait
Survey；
K repeats b and walks process, cleans the second syringe (14a)；
L drop replenishment control device (2) waits the beginning of next drop continuous micro-extraction process；
M is when the first piston (15) of the first syringe (14) arrives minimum capacity position, and drop replenishment control device (2) then controls
First motor (18) pulls the first syringe (14) extraction extract (7) to heap(ed) capacity.
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| CN108333011A (en) * | 2018-02-12 | 2018-07-27 | 云南中烟工业有限责任公司 | A kind of device of achievable sample high throughput processing |
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| CN117517696A (en) * | 2023-12-29 | 2024-02-06 | 杭州谱聚医疗科技有限公司 | System and sampling method for obtaining samples in situ on line |
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