CN208187827U - A kind of water sample preprocessing system - Google Patents
A kind of water sample preprocessing system Download PDFInfo
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- CN208187827U CN208187827U CN201820872127.6U CN201820872127U CN208187827U CN 208187827 U CN208187827 U CN 208187827U CN 201820872127 U CN201820872127 U CN 201820872127U CN 208187827 U CN208187827 U CN 208187827U
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Abstract
The utility model provides a kind of water sample preprocessing system, including sample injection unit, level-one liquid storage unit, second level liquid storage unit, enrichment unit and nitrogen blow upgrading unit;Sample injection unit includes funnel and water-supply-pipe interconnected, is provided with filter in water-supply-pipe;Water-supply-pipe is connected with level-one liquid storage unit;Second level liquid storage unit includes three or more device for storing liquid, enrichment unit includes three or more enriching columns, device for storing liquid passes through pipeline correspondingly with enriching column and valve is connected, and device for storing liquid entrance is provided with filter membrane, and device for storing liquid entrance is connected with level-one liquid storage unit by pipeline and valve;Enriching column blows enrichment facility with nitrogen and is connected.The system of the utility model is using simple, treatment effeciency is high, it can be required to complete pre-treatment work using different enrichment units according to water sample detection, the synchronous preceding processing realized to heterogeneity micropollutants in same reaction system, it significantly improves pre-treatment effect and reduces energy consumption, optimize structure of reactor, reduces occupied area.
Description
Technical field
The utility model belongs to water environment detection field, in particular to a kind of water sample preprocessing system.
Background technique
Since abuse and municipal sewage plant's prior art processing of various kinds of drug are not thorough, in recent years, all kinds of medicines
Object is frequently detected in the water sources such as rivers, lake, underground water, municipal wastewater, although its concentration mostly in ng/L to μ g/L,
But the long-term preservation of these substances may generate potential hazard to the ecosystem.Existing analysis instrument can not directly determine water sample
Amount detection needs to carry out pre-treatment to water sample.Therefore, the analysis and detection technology of environmental water sample is usually by Sample Pretreatment Technique
It is formed with instrumental quantitative analysis technology two parts.By water sample pretreatment technology, can the tested trace components of enrichment method, drop
Low detection limit, and the sensitivity of improvement method, and the high analysis instrument of efficient and sensible, adaptability ensure that the accurate of testing result
Property.Therefore, integrated water environment pre-processing device small in size, high-efficient, easy to operate and technology are always domestic and international water ring
A difficult point and research hotspot in border pre-treatment work.
Common environmental water sample pre-treatment side includes that liquid-liquid extraction, dispersive liquid-liquid microextraction, Solid Phase Extraction and solid phase are micro-
Extraction etc..However, liquid-liquid extraction is cumbersome, need to consume a large amount of solvents, it is at high cost, environmental pollution is caused, is absolutely recycled
Rate is relatively low;Dispersive liquid-liquid microextraction is affected by pH, and the selection of organic solvent is more demanding;Solid Phase Extraction is needed using solid
Phase extraction equipment and extraction pillar, it is at high cost;Solid phase microextraction, sensitivity is relatively low, need to find suitable derivatising condition.
Therefore, integrated pretreating device is designed, establishing one kind can carry out at normal temperatures and pressures, and have high efficiency and wide spectrum
Property water environment pretreatment technology, improve the timeliness of sample treatment, simplifying technique simultaneously reduces volume, before being effective solve efficiently
Processing problem and the technology is pushed to be capable of the key of practical application.
Utility model content
Purpose of utility model: the purpose of the utility model is to provide a kind of high-efficient, safety, wide spectrum is able to carry out field
The water sample pre-processing device of water body fast sampling concentration.
Technical solution: the utility model provides a kind of water sample preprocessing system, which includes sample introduction list
Member, level-one liquid storage unit, second level liquid storage unit, enrichment unit and nitrogen blow upgrading unit;Sample injection unit includes leakage interconnected
Bucket and water-supply-pipe are provided with filter in water-supply-pipe;Water-supply-pipe is connected with level-one liquid storage unit;Second level liquid storage unit includes three
The above device for storing liquid, enrichment unit include three or more enriching columns, device for storing liquid and enriching column pass through correspondingly pipeline and
Valve is connected, and device for storing liquid entrance is provided with filter membrane, and device for storing liquid entrance is connected with level-one liquid storage unit by pipeline and valve;
Enriching column blows upgrading unit with nitrogen and is connected.
Preferably, more medium filter and miillpore filter are disposed with along water sample flow direction in water-supply-pipe;Funnel and
The valve that can be used for controlling water speed is additionally provided between water-supply-pipe, water-supply-pipe includes polyfluortetraethylene pipe interconnected and water outlet
Hose, level-one liquid storage unit are provided with entrance and first outlet, and the entrance of level-one liquid storage unit is connected with water-supply-pipe, level-one liquid storage
The first outlet of unit is connected with second level liquid storage unit by pipeline and valve.
Wherein, the device for storing liquid main body in level-one liquid storage unit and second level liquid storage unit is respectively that can store the appearance of water sample
Device.The effect of above-mentioned filter and filter membrane is the insoluble matter and other impurity filtered out in water sample, and filter and filter membrane can bases
The physicochemical property of target contaminant is selected, it is preferable that is filtered in water-supply-pipe using the micropore that aperture is 0.22um~0.45um
Film, including ceramic microporous membranes, glass microporous film, all kinds of metal micro-holes films and cellulose esters microporous barrier;In second level liquid storage unit
Filter membrane be miillpore filter, it can be achieved that conventional field sampling filtering needs.The type of miillpore filter can be polluted according to contained by water body
Object and test request need to adjust, including ceramic microporous membranes, glass microporous film, all kinds of metal micro-holes films, cellulose esters;Into
One step preferably, in second level liquid storage unit, the filter membrane of device for storing liquid be respectively 0.45 μm cellulose acetate sheets, 0.7 μm
The glass fiber filter of glass fiber filter and 0.45 μm of aperture.Enriching column known in the art can be used in enriching column.
In addition, above-mentioned water sample preprocessing system further includes tail washings processing unit, for water sample extra in processing system.One
Grade liquid storage unit is additionally provided with second outlet, and the second outlet and tail washings processing unit of level-one liquid storage unit pass through pipeline and valve
It is connected.
Device for storing liquid in second level liquid storage unit is respectively arranged with entrance, first outlet and second outlet, device for storing liquid
Entrance is connected with the first outlet of level-one liquid storage unit by pipeline and valve, and first outlet and the enriching column of device for storing liquid pass through
Pipeline is connected with valve, and the second outlet of device for storing liquid is connected with tail washings processing unit by pipeline and valve.
Above-mentioned water sample preprocessing system further includes eluent storage unit, and eluent storage unit includes that multiple eluents are deposited
Storage bottle, multiple eluent holding bottles pass through pipeline and valve respectively and are connected with each enriching column, for conveying eluent for enriching column.
The selection for being enriched with column packing and filter membrane type and aperture can be according to the physicochemical property such as octanol of target enriched fractions
Whether water partition coefficient is configured by factors such as filter membrane absorption retentions.Specifically, enrichment unit includes perfluorooctanoic acid and complete
Fluorine octyl sulfonic acid enriching column, organic filters enriching column and antibiotic enriching column, it is parallel with one another between each enriching column, it is respectively independent
Work.Perfluorooctanoic acid and perfluoro octyl sulfonic acid enriching column are preferably Oasis WAX enriching column, and organic filters enriching column is preferred
For Oasis HLB enriching column, antibiotic enriching column is preferably Oasis HLB enriching column.In second level liquid storage unit, with perfluoro caprylic acid
The filter membrane for the device for storing liquid inlet that class and perfluoro octyl sulfonic acid enriching column are connected is preferably the acetate fiber that aperture is 0.45 μm
Plain filter membrane, the filter membrane for the device for storing liquid inlet being connected with organic filters enriching column are preferably the glass fibers that aperture is 0.7 μm
Filter membrane is tieed up, the filter membrane for the device for storing liquid inlet being connected with antibiotic enriching column is preferably the glass fibre filter in 0.45 μm of aperture
Film.
In addition, above-mentioned water sample preprocessing system further includes power unit, power unit includes vacuum pump and peristaltic pump, vacuum
Pump is connected with enriching column, for removing the residual moisture in enriching column;Peristaltic pump is connected with pipeline each in system, each for pumping
Water sample, eluting solvent etc., preferably multi-channel peristaltic pump in pipeline.
Electric energy can be used in the power source of this system;Preferably, solar panels, hydroelectric installation are additionally provided in system
And/or wind power generation plant, for providing electric power for the power device in system.
Above-mentioned valve is preferably solenoid valve, and is multidirectional control valve, can control system by the opening and closing of control valve
The flow direction of water sample, eluent and gas in system.
It is that existing nitrogen blows enrichment facility that above-mentioned nitrogen, which blows upgrading unit main body, specifically includes nitrogen evaporator, automatic conveying belt, holds
Platform and quantitative concentrating instrument.Upgrading unit independently is blown with nitrogen and is connect in the eluent outlet of enriching column.Preferably, it is single to blow concentration for nitrogen
Member further includes automatically or semi-automatically chromatogram bottle sealing machine, and the water sample for completing pre-treatment carries out sealing preservation, after being used for
Continuous chemical detection analysis.
The first outlet height of level-one liquid storage unit can be according to water sample in the different device for storing liquid of second level liquid storage unit
The needs of hydraulic detention time and sample volume are adjusted.
Also settable fluid flowmeter, check-valves and pressure sensor in second level liquid storage unit.In addition, the pre-treatment of this water sample
It further include the functions such as setting parameter, signal acquisition, analysis, simulation calculating, auto-control, false alarm, data record in system
Element, these elements use element known in the art.
The working principle of the utility model is: so that water sample to be processed is entered water-supply-pipe by funnel after acquisition wild water sample,
In water-supply-pipe, filter removes most of impurity in water sample;Then, water sample enters level-one liquid storage unit, is then stored up by level-one
Liquid unit enters the different device for storing liquid of second level liquid storage unit, and water sample filters before entering device for storing liquid through filter membrane again, removes
Unwanted compound in water sample;Then, water sample respectively enters different enrichments by the different device for storing liquid of second level liquid storage unit
Column after enriched and elution step, then blows enrichment facility with nitrogen and carries out quantitative concentration and collect, completes water sample variety classes trace
The pre-treatment of micropollutants works;Each section remaining liq is discharged after being focused on by tail washings processing unit.
The utility model has the advantages that the water sample preprocessing system of the utility model is using simple, treatment effeciency is high, can effectively, it is economical,
Environmental protection integrally passes through water process before primary filter, multi-stage diffluence progress sample, is required according to water sample detection using different
Enrichment unit completes pre-treatment work, and the synchronous preceding processing realized to heterogeneity micropollutants, shows in same reaction system
It writes and improves pre-treatment effect and reduce energy consumption, optimize structure of reactor, reduce occupied area.Specifically, the utility model with
The prior art is compared, and is had the following beneficial effects:
1, using the difference of variety classes contaminant trace species physicochemical property in natural practical water body, pass through the object of sample injection unit
Reason filtering and the specific aim enrichment elution concentration of different enrichment units, can handle before field is carried out in situ water sample, realize single
One technique or the unapproachable water sample test request of general technology, can also reduce pre-treatment cost, be completed at the same time to remaining water sample
Purification thoroughly, avoids generating secondary pollution, environmental protection is reliable, has a vast market foreground;
2, it using the multiple device for storing liquid and enriching column being arranged in parallel, can be polluted in same time synchronization implementation heterogeneity
The water sample pre-treatment time is shortened in the sampling of object, is reduced significantly reactor volume while improving treatment effect;Utilize different richnesses
Clustered column increases the diversity of pre-treatment, practical water body can be made to be filled in preprocessing system by multidirectional switching valve in system
Divide optimization and utilizes.
3, the setting of solar panel, wind power generation plant and hydroelectric installation can pass through cleaning in energy free
Water sample pre-treatment is rapidly completed in the energy;
4, using fluid flowmeter, pressure sensor, solenoid valve, Automatic Control Unit and automatic sealing, it can be achieved that processed
Full-automatic, the intelligentized control method of journey.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of water sample preprocessing system.
1- conical funnel;The controllable valve of 2- funnel bottle neck;3- more medium filter;4- polytetrafluoroethylene (PTFE) hard tube;5- is micro-
Hole filter membrane;6- delivery hose;7- eluent holding bottle;8- eluent holding bottle;9- eluent holding bottle;The storage of 10- eluent
Bottle;11- eluent holding bottle;12- eluent holding bottle;13- solenoid valve;14- solenoid valve;15- solenoid valve;16- solenoid valve;
17- automates water-level instrumentation;18- pressure gauge;19- solenoid valve;20- outlet valve;21- solenoid valve;22- fluid flowmeter;23-
Solenoid valve;24- fluid flowmeter;25- solenoid valve;26- fluid flowmeter;27- cellulose acetate sheets;28- pressure sensor;
29- water-level instrumentation;30- solenoid valve;The first device for storing liquid of 31-;32- solenoid valve;33- glass fiber filter;34- pressure sensing
Device;35- water-level instrumentation;36- solenoid valve;37- solenoid valve;The second device for storing liquid of 38-;39- glass fiber filter;40- pressure
Sensor;41- water-level instrumentation;42- solenoid valve;43- solenoid valve;44- third device for storing liquid;45- wind power generation plant;46-
Hydroelectric installation;47- vacuum pump;48- peristaltic pump;49- solenoid valve;50- solenoid valve;The first enriching column of 51-;52- pressure passes
Sensor;53- water-level instrumentation;54- three-way valve;55- solenoid valve;The second enriching column of 56-;57- pressure sensor;58- water level
Monitor;59- three-way valve;60- solenoid valve;61- third enriching column;62- pressure sensor;63- water-level instrumentation;64- tri-
Port valve door;65- total valve;66- water-level gauge;67- degraded layer;68- pressure gauge;69- water discharging valve;70- nitrogen evaporator;71- is automatic
Conveyer belt;72- cushion cap;73- quantifies concentrating instrument;74- solenoid valve;75- solenoid valve;76- solenoid valve;77- solar panels.
Specific embodiment
As shown in Figure 1, water sample preprocessing system includes sample injection unit, level-one liquid storage unit, second level liquid storage unit, enrichment list
Member, eluent storage unit, nitrogen blow upgrading unit, tail washings processing unit and power unit.
Sample injection unit includes that conical funnel 1, the controllable valve 2 of funnel bottle neck, more medium filter 3, polytetrafluoroethylene (PTFE) are hard
Pipe 4, miillpore filter 5 and delivery hose 6.Wherein, conical funnel 1, polytetrafluoroethylene (PTFE) hard tube 4 and delivery hose 6 are sequentially connected,
More medium filter 3 and miillpore filter 5 are disposed in polytetrafluoroethylene (PTFE) hard tube 4.More medium filter 3 include cartridge filter and
Filtering metal sieve, for removing visible foreign in water removal;Miillpore filter 5 is the miillpore filter that aperture is 0.22um~0.45um, can
Ceramic microporous membranes, glass microporous film, all kinds of metal micro-holes films or cellulose esters microporous barrier are thought, for further fine removal
Visible foreign.
The main part of level-one liquid storage unit is the container for accommodating water sample, in addition, level-one liquid storage unit further includes setting
Set automation water-level instrumentation 17 and pressure gauge 18 on container.Level-one liquid storage unit is provided with entrance, first outlet and
Two outlets, the entrance of level-one liquid storage unit connect delivery hose 6, are provided with solenoid valve at the first outlet of level-one liquid storage unit
19, the first outlet of level-one liquid storage unit connects second level liquid storage unit;Water outlet is provided at the second outlet of level-one liquid storage unit
Valve 20, second outlet connect tail washings processing unit.
Second level liquid storage unit includes the first device for storing liquid 31, the second device for storing liquid 38 and third device for storing liquid 44.Level-one storage
The first outlet of liquid unit by pipeline respectively with 44 phase of the first device for storing liquid 31, the second device for storing liquid 38 and third device for storing liquid
Even.Wherein, it is provided with solenoid valve 21 and fluid flowmeter 22 in the pipeline of connection level-one liquid storage unit and the first device for storing liquid 31,
It is provided with solenoid valve 23 and fluid flowmeter 24 in the pipeline of connection level-one liquid storage unit and the second device for storing liquid 38, connects level-one
Solenoid valve 25 and fluid flowmeter 26 are provided in the pipeline of liquid storage unit and third device for storing liquid 44.
First device for storing liquid 31, the second device for storing liquid 38 and third device for storing liquid 44 are respectively arranged with entrance, first outlet
And second outlet.First device for storing liquid, 31 inlet is provided with the cellulose acetate sheets 27 in 0.45 μm of aperture, the first liquid storage dress
It sets 31 and is connected by being provided with the pipeline of solenoid valve 74 with power unit, be provided with electricity at the first outlet of the first device for storing liquid 31
Magnet valve 30 is provided with solenoid valve 50 at the second outlet of first device for storing liquid 31, and the second outlet of the first device for storing liquid 31 passes through
Pipeline is connected with tail washings processing unit.Second device for storing liquid, 38 inlet is provided with the glass fiber filter 33 in 0.7 μm of aperture, the
Two device for storing liquid 38 are connected by being provided with the pipeline of solenoid valve 75 with power unit, at the first outlet of the second device for storing liquid 38
It is provided with solenoid valve 36, is provided with solenoid valve 55 at the second outlet of the second device for storing liquid 38, the second of the second device for storing liquid 38
Outlet is connected by pipeline with tail washings processing unit.44 inlet of third device for storing liquid is provided with the glass fibre in 0.45 μm of aperture
Filter membrane 39, third device for storing liquid 44 are connected by being provided with the pipeline of solenoid valve 76 with power unit, third device for storing liquid 44
It is provided with solenoid valve 42 at first outlet, solenoid valve 60, third liquid storage dress are provided at the second outlet of third device for storing liquid 44
44 second outlet is set to be connected by pipeline with tail washings processing unit.Pressure sensor 28 is additionally provided in first device for storing liquid 31
With water-level instrumentation 29, pressure sensor 34 and water-level instrumentation 35, third liquid storage dress are additionally provided in the second device for storing liquid 38
It sets and is additionally provided with pressure sensor 40 and water-level instrumentation 41 in 44.
Enrichment unit includes the first enriching column 51 (perfluorooctanoic acid and perfluoro octyl sulfonic acid enriching column), the second enriching column 56
(organic filters enriching column), third enriching column 61 (antibiotic enriching column), the 4th device for storing liquid, the 5th device for storing liquid and the 6th
Device for storing liquid.Wherein, the 4th device for storing liquid is arranged below the first enriching column 51, washes for perfluorooctanoic acid and perfluoro octyl sulfonic acid
De- liquid interposer, for temporarily storing the elution solution of the first enriching column 51;5th device for storing liquid is arranged in the second enriching column 56
Lower section is organic filters eluent interposer, for temporarily storing the elution solution of the second enriching column 56;6th device for storing liquid
It is arranged below third enriching column 61, is antibiotic eluent interposer, the elution for temporarily storing third enriching column 61 is molten
Liquid.Eluent storage unit includes eluent holding bottle 7, eluent holding bottle 8, eluent holding bottle 9, eluent holding bottle
10, eluent holding bottle 11 and eluent holding bottle 12.Eluent storage unit by total pipeline and three subtubes respectively with
First enriching column 51, the second enriching column 56 are connected with third enriching column 61, wherein it is provided with solenoid valve 13 in total pipeline, three
Subtube is respectively arranged with solenoid valve 14,15,16.First enriching column, the 51 entrance first outlet with the first device for storing liquid 31 respectively
And eluent storage unit is connected, 51 exit lower end of the first enriching column is provided with the 4th device for storing liquid, in the 4th device for storing liquid
It is provided with pressure sensor 52 and water-level instrumentation 53, the 4th device for storing liquid lower end exit is provided with solenoid valve 54;Second is rich
56 entrance of clustered column is connected with the first outlet of the second device for storing liquid 38 and eluent storage unit respectively, and the second enriching column 56 goes out
Mouthful lower end is provided with the 5th device for storing liquid, is provided with pressure sensor 57 and water-level instrumentation 58 in the 5th device for storing liquid, and the 5th
Device for storing liquid lower end exit is provided with solenoid valve 59;61 entrance of third enriching column goes out with the first of third device for storing liquid 44 respectively
Mouth and eluent storage unit are connected, and 61 exit lower end of third enriching column is provided with the 6th device for storing liquid, the 6th device for storing liquid
In be provided with pressure sensor 62 and water-level instrumentation 63, the 6th device for storing liquid lower end exit is provided with solenoid valve 64.4th
Upgrading unit and tail washings are blown by pipeline and nitrogen respectively in device for storing liquid, the 5th device for storing liquid and the outlet of the 6th device for storing liquid lower end
Processing unit is connected.Each enriching column is realized by the control of solenoid valve 21,23 and 25 and is worked independently.
Be provided with total valve 65 in the pipeline of end entrance on connection tail washings processing unit, total valve 65 respectively with level-one liquid storage
The second outlet of unit and the first device for storing liquid 31, the second device for storing liquid 38, third device for storing liquid 44, the 4th device for storing liquid,
5th device for storing liquid and the outlet of the 6th device for storing liquid lower end are connected.Tail washings processing unit is provided with water-level gauge 66, degraded layer 67, pressure
Power table 68 and water discharging valve 69, degraded layer 67 include materials, untreated water sample and the elutions such as microorganism, active carbon, gravel, cobble
Liquid is discharged after the processing of tail washings device.
It includes nitrogen evaporator 70, automatic conveying belt 71, cushion cap 72 and quantitative concentrating instrument 73 that nitrogen, which blows enrichment facility,.
The electric power of vacuum pump 47 and peristaltic pump 48 can be provided by typical power system, can also be by solar panels 77, wind-force
Power generator 45, hydroelectric installation 46 are provided by USB interface, it is preferable that solar panels 77 can be installed on this system
Side and top, wind power generation plant 45 are mounted on the device surrounding of this system, and hydroelectric installation 46 is mounted on this system
Bottom, USB interface are mounted on side.
In actual work, after the completion of acquiring wild water sample, water sample to be processed is added in funnel 1, water sample is in vacuum pump
Primary filtration processing is carried out through more medium filter and miillpore filter under 47 suction filtration effect, is controlled by the controllable valve 2 of bottle neck
Water sample enters the speed of polytetrafluoroethylene (PTFE) hard tube 4, enters level-one liquid storage unit using hose 6, opens solenoid valve 19, pass through stream
Meter monitors water speed, guarantees that water sample speed is stored in 100ml/min or so or Reasonable Speed, flows out from level-one liquid storage unit,
It has respectively entered in the first device for storing liquid 31, the second device for storing liquid 38 and third device for storing liquid 44, then enters back into the first enrichment
Column 51 (perfluorooctanoic acid and perfluoro octyl sulfonic acid enriching column), the second enriching column 56 (organic filters enriching column), third enrichment
In column 61 (antibiotic enriching column), after filtering, enrichment and elution step, then enrichment facility is blown with nitrogen and carries out quantitative concentration and receipts
Collection completes the pre-treatment work of water sample variety classes trace micropollutants.Remaining liq through each device can be handled by tail washings
Device centralized processing.
Specifically, when being enriched with using enriching column 51 to perfluorochemical, solenoid valve 19 and 21, water sample warp are opened
The cellulose acetate sheets 27 in 0.45 μm of aperture enter the first device for storing liquid 31 after filtering;Solenoid valve 13,14 and 32 is opened, to
Oasis WAX enriching column 51 is successively with 4mL 0.1% (V/V) ammonia-methanol solution in eluent holding bottle 7, eluent storage
After 4mL ultrapure water activation in 4mL methanol solution and eluent holding bottle 9 in bottle 8, solenoid valve 13 and 14 is closed, is then beaten
Open electromagnetic valve 30 makes the water sample in the first device for storing liquid 31 flow into Oasis WAX enriching column 51, controls water sample speed in 5mL/
Min, while to the 50ng/mL inner mark solution 13C8-PFOA of 100 μ L of the addition of enriching column 51, the perfluorochemical being enriched in water sample;
Three-way valve 54 is opened, 30min is taken out with vacuum pump 47, the residual moisture of Oasis WAX enriching column 51 is completely removed, is then beaten
Valve opening door 13 and 14, respectively in 4mL0.1% (V/V) ammonia-methanol solution and eluent holding bottle 8 in eluent holding bottle 7
4mL methanol solution eluted, elution speed keeps 1mL/min, and eluent respectively enters corresponding eluent interposer, just
Constant volume is blown in the nitrogen of next step.
When being enriched with using the second enriching column 56 to organic filters, valve 19 and 23 is opened, water sample is through 0.7 μm of hole
The glass fiber filter 33 of diameter enters the second device for storing liquid 38 after filtering;Solenoid valve 13,15 and 37 is opened, it is rich to Oasis HLB
Methanol of the clustered column 56 successively with the dichloromethane solution of the 6mL in eluent holding bottle 10,6mL in eluent holding bottle 8 is molten
After the activation of the ultrapure water of liquid and the 6mL in eluent holding bottle 9, solenoid valve 13 and 15 is closed;Then solenoid valve 36 is opened, makes the
Water sample in two device for storing liquid 38 flows into Oasis HLB enriching column 56, controls water sample speed in 10mL/min;Simultaneously to enriching column
56 are added the 100ng/mL organic filters mixing internal standard compound of 100 μ L, the organic filters being enriched in water sample;Open three-way valve
59,30min is taken out with vacuum pump 47, the residual moisture of Oasis HLB enriching column 56 is completely removed, then uses 1: 1 (V/ of 10mL
V) dichloro methane-methanol is eluted, and elution speed keeps 2mL/min.
When being enriched with using third enriching column 61 to the antibiotic in water sample, valve 19 and 25, water sample warp are opened
The glass fiber filter 39 in 0.45 μm of aperture enters third device for storing liquid 44 after filtering;Solenoid valve 13,16 and 43 is opened, to
Oasis HLB enriching column 61 is successively with the methanol solution of the 5mL in eluent holding bottle 8 and the 5mL in eluent holding bottle 9
After ultrapure water activation, solenoid valve 13 and 16 is closed, opens solenoid valve 42, water sample is made to flow into third enrichment from third device for storing liquid 44
Column 61, control water sample speed are added the antibiotic mixing internal standard compound of 100 μ L 50ng/mL in 5mL/min, are enriched in water sample
Antibiotic;Three-way valve 64 is opened, 30min is taken out with vacuum pump 47, the residual moisture of Oasis HLB enriching column 61 is gone completely
It removes, is then eluted with 6mL methanol and 6mL methanol/acetone (11) (v: v=1: 1), elution speed keeps 2mL/min.
Three-way valve 54,59 and 64 is opened, it can be respectively by the first enriching column 51, the second enriching column 56, third enriching column 61
Eluent be slowly blown to mild nitrogen net dry, residue methanol dissolve and is settled to 1mL, and collection is in 1.5mL brown color
It composes in bottle, in case target contaminant chemical detection is analyzed.
Claims (8)
1. a kind of water sample preprocessing system, which is characterized in that the water sample preprocessing system includes sample injection unit, level-one liquid storage list
Member, second level liquid storage unit, enrichment unit and nitrogen blow upgrading unit;The sample injection unit includes funnel interconnected and water delivery
It manages, is provided with filter in the water-supply-pipe;The water-supply-pipe is connected with the level-one liquid storage unit;The second level liquid storage unit
Including three or more device for storing liquid, the enrichment unit includes three or more enriching columns, the device for storing liquid and the enriching column
It is connected correspondingly by pipeline with valve, the device for storing liquid entrance is provided with filter membrane, the device for storing liquid entrance and institute
Level-one liquid storage unit is stated to be connected by pipeline with valve;The enriching column blows enrichment facility with the nitrogen and is connected.
2. water sample preprocessing system according to claim 1, which is characterized in that in the sample injection unit, the funnel and
Valve is additionally provided between water-supply-pipe;The water-supply-pipe includes polyfluortetraethylene pipe and delivery hose interconnected, described defeated
More medium filter and miillpore filter are disposed with along water sample flow direction in water pipe.
3. water sample preprocessing system according to claim 1, which is characterized in that the level-one liquid storage unit is provided with entrance
And first outlet, the entrance of the level-one liquid storage unit are connected with the water-supply-pipe, the first outlet of the level-one liquid storage unit
It is connected with the second level liquid storage unit by pipeline and valve.
4. water sample preprocessing system according to claim 3, which is characterized in that the water sample preprocessing system further includes tail washings
Processing unit, the level-one liquid storage unit are additionally provided with second outlet, the second outlet of the level-one liquid storage unit and the tail
Liquid processing unit is connected by pipeline with valve.
5. water sample preprocessing system according to claim 4, which is characterized in that in the second level liquid storage unit, liquid storage dress
It installs and is equipped with entrance, first outlet and second outlet, the entrance of the device for storing liquid goes out with the first of the level-one liquid storage unit
Mouth is connected by pipeline with valve, and the first outlet of the device for storing liquid is connected with the enriching column by pipeline and valve, institute
The second outlet for stating device for storing liquid is connected with the tail washings processing unit by pipeline and valve.
6. water sample preprocessing system according to claim 1, which is characterized in that the water sample preprocessing system further includes elution
Liquid storage unit, the eluent storage unit include multiple eluent holding bottles, and the multiple eluent holding bottle leads to respectively
Piping and valve are connected with the enriching column.
7. water sample preprocessing system according to claim 1, which is characterized in that the water sample preprocessing system further includes power
Unit, the power unit include vacuum pump and peristaltic pump, and the vacuum pump is connected with the enriching column, the peristaltic pump and institute
Water-supply-pipe is stated to be connected.
8. water sample preprocessing system according to claim 1, which is characterized in that it includes that nitrogen is blown that the nitrogen, which blows enrichment facility,
Instrument, automatic conveying belt, cushion cap and quantitative concentrating instrument.
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