CN111442966A - In-situ extraction, enrichment and sampling device and method for organic pollutants in seawater - Google Patents
In-situ extraction, enrichment and sampling device and method for organic pollutants in seawater Download PDFInfo
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- CN111442966A CN111442966A CN202010267990.0A CN202010267990A CN111442966A CN 111442966 A CN111442966 A CN 111442966A CN 202010267990 A CN202010267990 A CN 202010267990A CN 111442966 A CN111442966 A CN 111442966A
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- 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
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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G01N1/405—Concentrating samples by adsorption or absorption
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Abstract
The invention belongs to the technical field of marine environment investigation, and particularly relates to an in-situ extraction, enrichment and sampling device and method applied to seawater organic pollutants. An in-situ extraction, enrichment and sampling device for organic pollutants in seawater comprises a sample extraction and enrichment unit, a sample introduction unit, a drainage unit, a pressure balance unit, a sample elution unit, a sample transfer unit and a control circuit board assembly; the sample introduction unit, the water drainage unit, the pressure balance unit, the sample elution unit and the sample transfer unit are all connected with the sample extraction and enrichment unit, and all the units are controlled by the control circuit board assembly to finish sample introduction, extraction and enrichment of organic pollutants in seawater. The device and the method of the invention adopt multiple sample injection, thereby improving the enrichment multiple of the target pollutants. After each sample introduction, the nano particles are fully contacted and mixed with the seawater sample through stirring, so that the extraction efficiency is improved, and the underwater in-situ extraction, enrichment and sampling of organic pollutants are realized.
Description
Technical Field
The invention belongs to the technical field of marine environment investigation, and particularly relates to an in-situ extraction, enrichment and sampling device and method applied to seawater organic pollutants.
Background
Polycyclic Aromatic Hydrocarbons (PAHs) are persistent organic pollutants having two or more benzene rings and widely exist in the environment. Organic pollutants in marine environments mainly come from paths such as oil leakage, sewage discharge, atmospheric sedimentation and surface runoff, and the pollutants are easily accumulated in marine organisms such as fish and shellfish and finally affect human health through a food chain. In recent years, with the aggravation of marine pollution, people pay more and more attention to the monitoring of PAHs.
In addition, the samples need to be subjected to complex extraction and concentration treatment before laboratory analysis, and the traditional pretreatment processes (liquid-liquid extraction (LL E), solid-phase extraction (SPE) and the like) have the problems of large dosage of eluent, easy blockage of an extraction column and the like and have larger time lag.
Disclosure of Invention
The invention provides an in-situ extraction, enrichment and sampling device for organic pollutants in seawater, aiming at solving the problems of the existing underwater in-situ extraction, enrichment and monitoring technology.
The technical scheme adopted by the invention for solving the technical problems is as follows: an in-situ extraction, enrichment and sampling device for organic pollutants in seawater comprises a sample extraction and enrichment unit, a sample introduction unit, a drainage unit, a pressure balance unit, a sample elution unit, a sample transfer unit and a control circuit board assembly; the sample introduction unit, the water drainage unit, the pressure balance unit, the sample elution unit and the sample transfer unit are all connected with the sample extraction and enrichment unit, and all the units are controlled by the control circuit board assembly to finish sample introduction, extraction and enrichment of organic pollutants in seawater.
As a preferred mode of the invention, the sample extraction and enrichment unit mainly comprises a sample processing tank, a stirring motor and a stirring frame; the sample processing tank is provided with a plurality of interfaces, and the interfaces are used for connecting other units; the stirring motor is arranged on the sample processing tank through an interface and is connected with a stirring frame in the sample processing tank; the bottom end in the sample processing tank is provided with a conical closing-in; and a sample elution cavity is arranged below the conical closing-in.
Further preferably, the stirring frame consists of a cylindrical sealing shaft, an annular plate type structure and a spiral shaft; the cylindrical sealing shaft is arranged at the top of the annular plate type structure, and the spiral shaft is arranged at the bottom of the annular plate type structure; the spiral direction of the spiral shaft is from bottom to top; the lower part of the annular plate type structure is conical and is attached to the conical closing-in of the sample processing tank.
Further preferably, the inner wall of the sample processing tank is coated with a teflon coating.
As another preferred mode of the invention, the sample injection unit mainly comprises a first flow meter, a first electric ball valve and a first water pump; the water outlet of the first water pump is connected with an interface on the sample processing tank through a pipeline; the pipeline is sequentially connected with a first electric ball valve and a first flowmeter.
Further preferably, the head of the first water pump is provided with a filter cover which wraps the water inlet
Further preferably, the control circuit board assembly monitors the signal of the first flowmeter, and when a set value is reached, the first electric ball valve and the first water pump are closed.
As another preferable mode of the present invention, the drainage unit mainly comprises a second flowmeter, a second electric ball valve, a second water pump and a filter screen; the filter screen is arranged in the interface of the sample processing tank and is tightly attached to the interface; the second water pump is connected with the interface of the sample processing tank through a pipeline, and a second electromagnetic valve and a second flowmeter are sequentially connected to the pipeline.
Further, the control circuit board assembly monitors signals of the second flowmeter, and when no signal is output, the second electric ball valve and the second water pump are closed.
As another preferred mode of the invention, the pressure balancing unit mainly comprises a balancing gas tank, a balancing plug and an anti-drop cover; the balance gas tank is a container with a bottom, and the bottom is provided with a vent hole; the vent hole is connected with the interface of the sample processing tank through a pipeline; the anti-drop cover is arranged at the top of the balance gas tank; the balance plug is arranged in the balance gas tank and moves up and down in the balance gas tank along with the change of external water pressure or internal air pressure.
As another preferred mode of the present invention, the sample elution unit comprises a first electric push rod, a first syringe, a one-way valve; the tail part of a piston rod of the first syringe is connected with the first electric push rod, and the interior of the first syringe is filled with eluent in advance; the head of the first injector is connected with the one-way valve through a polytetrafluoroethylene liquid pipe; the one-way valve terminal is connected with the interface of the sample processing tank through a pipeline, and the opening direction of the one-way valve points to the sample processing tank from one end of the injector.
As another preferred mode of the present invention, the sample transfer unit comprises an adapter, a multi-way valve, a sampling bottle, a second electric push rod, and a second syringe; one path of the multi-way valve is connected with an outlet of the sample elution cavity through a joint; one path is connected with the injection end of the second injector through a polytetrafluoroethylene liquid pipe, and the other path is connected with a liquid discharge pipe; at least one path is connected with a sampling bottle; the tail part of a piston rod of the second injector is connected with a second electric push rod; the second electric push rod is controlled by the control circuit board assembly.
Furthermore, the device also comprises a pressure sensor, and the pressure sensor is used for acquiring the pressure value of the water depth where the device is located.
An in-situ extraction, enrichment and sampling method for organic pollutants in seawater comprises the following steps:
(1) taking sufficient functionalized nano particles, and filling the sufficient functionalized nano particles into the inner cavity of the sample treatment tank in advance;
(2) injecting a seawater sample into the sample treatment tank;
(3) stirring at a high speed to ensure that the nano particles are fully contacted with the seawater sample to complete the extraction of the target substance; discharging the seawater through a drainage unit;
(4) repeating the steps (2) and (3) for multiple times to realize the enrichment of the target substance;
(5) injecting the eluent into a sample treatment tank, stirring at low speed to ensure that the nano particles are fully contacted with the eluent, and finishing desorption of the target substance;
(6) transferring the eluent obtained in the step (5) into a sample bottle through a sample transfer unit to finish sampling.
Compared with the prior art, the invention has the advantages and beneficial effects that: the invention provides a solution integrating in-situ sampling, extraction and enrichment functions specially for trace organic pollutants in seawater, the whole process is completed underwater in situ, and finally a highly concentrated sample is obtained and can be seamlessly linked with gas-liquid phase analysis equipment in a laboratory. The scheme provides a whole-process automatic control solution idea of the seawater sampling and target pollutant extraction and enrichment process. The sampling process adopts a closed-open-closed mode, and the problem of cross contamination among different water layers in the submergence process of the sampling device is effectively solved. The water depth sensor is matched, so that sample collection of any target water level can be realized, the in-situ pollution condition can be truly reflected, and the seawater depth sensor is very favorable for seawater profile investigation. In addition, the method has the advantages that the particle size of the nanoparticles is small, the specific surface area is large, target substances can be extracted in a targeted manner after modification and functionalization treatment, the extraction time is short, the efficiency is high, and the problems of extraction column blockage, fiber breakage and the like in a conventional extraction mode are solved. The in-situ extraction, enrichment and sampling device for the organic pollutants can fill up the domestic blank, provides special equipment for marine scientific investigation, and has wide application prospect.
Drawings
FIG. 1 is an overall appearance diagram of an embodiment of the method for in-situ extraction, enrichment and sampling of organic pollutants in seawater according to the present invention;
FIG. 2 is a partial cross-sectional structural view;
FIG. 3 is a schematic view of the connection of the internal major components of FIG. 1 with the housing removed;
FIG. 4 is a schematic diagram of the construction of a sample processing tank;
FIG. 5 is a schematic view of the construction of the mixing frame;
FIG. 6 is a flowchart illustrating the operation of an embodiment of the method for in-situ extraction, enrichment and sampling of organic contaminants in seawater according to the present invention; wherein the reference numerals are as follows:
1. a sample processing tank; 2. sealing the shell; 3. a control circuit board assembly; 4. a third electric ball valve; 5. a balance gas tank; 6. a balance plug; 7. an anti-drop cover; 8. a first flow meter; 9. a first electrically powered ball valve; 10. a first water pump; 11. a filter housing; 12. a stirring motor; 13. a stirring frame; 14. a filter screen; 15. a filtration membrane; 16. an adapter; 17. a multi-way valve; 18. a sampling bottle; 19. a first electric push rod; 20. a first syringe; 21. a one-way valve; 22. a second electric push rod; 23. a second syringe; 24. a pressure sensor; 25. the water-tight connector, 26, a lifting ring, 27, a second flowmeter, 28, a second electric ball valve, 29, a second water pump and 30, a drain pipe.
Detailed Description
In order to facilitate an understanding of the invention, the invention is described in more detail below with reference to the accompanying drawings and specific examples. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
In order to reduce the workload of sampling and transporting organic pollutant samples in seawater, truly reflect the pollution condition of a target water level and meet the requirements of subsequent laboratory analysis equipment, the embodiment provides the sampling device for in-situ extraction and enrichment in seawater, and finally obtains a high-enriched sample with a small volume by adopting a method for extracting and enriching target substances in seawater by using nano particles and a series of processing means such as sampling, stirring, elution and the like in a closed-open manner.
The first embodiment provided by the invention is as follows: a device for in-situ extraction, enrichment and sampling of organic pollutants in seawater.
As shown in fig. 2 and 3, the device for in-situ extraction, enrichment and sampling of organic pollutants in seawater (hereinafter referred to as enrichment and sampling device) of the embodiment mainly comprises a sample extraction and enrichment unit, a sample introduction unit, a drainage unit, a pressure balance unit, a sample elution unit, a sample transfer unit, a control circuit board assembly, a sealed shell, a pressure sensor, a watertight connector, and the like.
The sample extraction and enrichment unit mainly comprises a sample processing tank 1, a stirring motor 12 and a stirring frame 13.
Wherein, the sample processing tank 1 is a cylindrical hollow container, as shown in fig. 4, a balance gas interface 101, a sample inlet 102, a sample outlet 103, and an eluent inlet 106 are sequentially arranged on the sidewall of the sample processing tank 1; the top of sample processing jar 1 is equipped with agitator motor connector 104, and the bottom sets up sample elution chamber 107, and the lower extreme in sample elution chamber 107 sets up adapter installing port 108. The balance gas interface 101, the sample inlet 102 and the eluent inlet 106 are all communicated with the inner cavity of the sample processing tank 1.
In addition, the bottom end in the sample processing tank 1 is provided with a conical closing-in 105, and the lower end of the conical closing-in 105 is connected with the upper end of the sample elution cavity 107, so that the sample collection is facilitated. Sample outlet 103 communicates with the upper end of sample elution chamber 107.
The stirring frame 13 is arranged in the inner cavity of the sample processing tank 1 and is connected with the stirring motor 12 through a stirring motor connecting port 104. The agitator motor 12 is located at the top of the sample processing tank 1.
In this embodiment, the structure of the stirring frame 13 is as shown in fig. 5, and the top thereof is a cylindrical sealing shaft 131 provided with a sealing ring mounting groove; the middle part is a section of annular plate-type structure 130 which is jointed with the conical closing-in 105 structure in the sample processing tank 1; the lower part is a section of spiral column 132, and the spiral column 13 is arranged at the center of the bottom of the annular plate-type structure 130, and the spiral direction is from the bottom to the top.
In this embodiment, the sample extraction and enrichment unit mainly provides a space for storing, extracting, and desorbing the target substance for the seawater sample. During operation, the inner cavity of the sample processing tank 1 is filled with enough functionalized nano particles in advance. After the seawater sample enters the inner cavity, the seawater sample and the inner cavity are fully contacted and mixed in a stirring mode, and the adsorption of a target substance is completed. In order to prevent the adhesion and residue of target pollutants, the inner cavity of the sample processing tank 1 is coated with Teflon.
The sample introduction unit mainly comprises a first flowmeter 8, a first electric ball valve 9, a first water pump 10 and a filter cover 11. The filter housing 11 is installed at the head of the first water pump 10 to cover the water inlet thereof. The filter mantle 11 circumference is equipped with the vertical retort of strip, effectively filters debris and the great granule in the water.
The water outlet of the first water pump 10 is connected with the sample inlet 102 through a pipeline, and a first electric ball valve 9 and a first flowmeter 8 are sequentially mounted on the pipeline.
First electronic ball valve 9, the control of control circuit board assembly 3, both ends are equipped with the installation internal thread, with pipeline threaded connection, adopt 316L stainless steel.
The first flowmeter 8 is an electromagnetic induction flowmeter and is used for measuring the volume of sample introduction, and mounting external threads are arranged at two ends of the flowmeter.
The sample introduction unit is mainly powered by a water pump, and an electric ball valve is used for realizing the on-off of a pipeline; the flow meter records the volume of the seawater sample as the calculation basis of the enrichment times. When the volume calculated by the flowmeter reaches a preset value, the control circuit board assembly 3 can further turn off the first water pump 10 and the first electric ball valve 9 in sequence according to the feedback signal of the first flowmeter 8.
The drainage unit mainly comprises a second flowmeter 27, a second electric ball valve 28, a second water pump 29 and a filter screen 14. Wherein, the filter screen 14 is a hollow cylinder structure, is installed inside the sample elution cavity 107, and is tightly attached to the inner wall thereof, so as to prevent the nano particles from being discharged along with the water flow in the drainage process.
The second water pump 29 is connected to the sample outlet 103 via a pipe, and a second electric ball valve 28 and a second flow meter 27 are mounted on the pipe in this order.
The second electric ball valve 28 is controlled by the control circuit board assembly 3, and two ends of the second electric ball valve are provided with mounting internal threads which are connected with the pipeline threads and made of 316L stainless steel.
The second flow meter 27 is an electromagnetic induction flow meter for measuring the volume of the sample, and has mounting external threads at both ends. The control circuit board assembly 3 monitors the signal of the second flowmeter 27, and when no signal is output, the second water pump 29 and the second electric ball valve 28 are sequentially closed.
The pressure balancing unit is used for keeping the internal pressure and the external pressure of the sample processing tank 1 equal, so that the sample feeding and the water discharging processes are smoothly carried out. Comprises a third electric ball valve 4, a balance gas tank 5, a balance plug 6 and an anti-drop cover 7. The balance gas tank 5 is a round pipe structure with a bottom, and the bottom is provided with a vent hole. The vent is connected to the balance gas port 101 of the sample processing tank 1 through a pipe.
The pressure balance unit is used for keeping the pressure balance inside and outside the sample processing tank 1 of the sample extraction and enrichment unit during sampling. The extraction enrichment sampling device is placed at a certain water depth, and the external pressure of the sample treatment tank 1 is certainly greater than the internal pressure. Along with the change of pressure, the balance plug 6 floats, and pressure is balanced, so that the sampling and drainage processes are smoothly carried out. Furthermore, the pressure equalization unit may save more water storage space for the sample processing tank 1.
The sample elution unit consists of a first electric push rod 19, a first syringe 20 and a one-way valve 21. The tail part of the piston rod of the first injector 20 is connected with the first electric push rod 19, and the interior of the first injector is filled with eluent in advance for eluting the target substance adsorbed by the nano particles. The injection end of the injector is connected with the one-way valve 21 through a polytetrafluoroethylene liquid tube. The opening direction of the one-way valve 21 is directed from one end of the syringe to the sample processing tank 1, and the terminal end thereof is directly connected to the eluent inlet 106 through a pipe.
The first electric push rod 19 is operated by the control circuit board assembly 3, 12V power supply is adopted, the stroke is 50mm, and the propelling speed is 5 mm/s.
The sample elution unit mainly completes the functions of storing the eluent and adding the eluent into the inner cavity of the sample processing tank 1.
The sample transfer unit comprises a filter membrane 15, an adapter 16, a multi-way valve 17, a sampling bottle 18, a second electric push rod 22 and a second injector 23. The filtering membrane 15 is in a circular sheet shape and made of titanium alloy material. Is mounted to the bottom of the adapter mounting opening 108 and is compressed by the adapter 16. One end of the adapter 16 is provided with external threads, the other end is a pagoda interface, and the axis is provided with a liquid channel.
The multi-way valve 17 is at least 5 ways, one way is connected with the external thread of the adapter 16 through a polytetrafluoroethylene liquid pipe, one way is connected with the second injector 23 through the polytetrafluoroethylene liquid pipe, and the other way is connected with the liquid discharge pipe 30. The other two paths are respectively connected with a sampling bottle 18. The tail part of a piston rod of a second injector 23 is connected with a second electric push rod 22, and the injection end of the injector is connected with the multi-way valve 17 through a polytetrafluoroethylene liquid pipe. The second electric push rod 22 is powered by 12V, the stroke is 50mm, and the working speed is 5 mm/s. The second electric push rod 22 is controlled to reciprocate by the control circuit board assembly 3, so that the second injector 23 is pulled and pushed, and the residual sample or the eluent is transferred.
The sample transfer unit is mainly used for transferring the desorbed eluent into a sampling bottle.
The pressure sensor 24 adopts an MS5837-30BA chip, adopts a 316L stainless steel shell, is encapsulated by epoxy resin, measures the water depth to 300m, monitors and controls the target water depth by adopting the pressure sensor, mutually transmits information with a shore-based control box, and is matched with an electric ball valve, a water pump and other execution components to realize a water sampling mode of closing and opening the sampling device, so that the cross contamination in the lowering process can be effectively reduced while the sampling requirement of any target water level is met, and the pollution condition of an in-situ water sample is truly reflected.
In this embodiment, since the apparatus needs to be lowered into the sea, in order to ensure the proper operation of the unit instrument parts, the unit instrument parts are placed 4 in the sealed housing 2. The water pump, the balance gas tank and the pressure sensor are positioned outside the sealed shell. The sealed case 2 is provided with a hanging ring 26 and a watertight connector 25. The hanging ring is used for facilitating the throwing of the device. As shown in fig. 1.
The second embodiment of the present invention is: a method for in-situ extraction, enrichment and sampling of organic pollutants in seawater. The process flow for the method is shown in fig. 6 in combination with the enrichment device shown in fig. 1 to 5, and comprises the following steps:
s601, preparation work.
A sufficient amount of functionalized nanoparticles is weighed and pre-filled into the sample processing tank 1.
The device is powered on, the control circuit board assembly 3 outputs an instruction, the third electric ball valve 4 is opened, and the first electric ball valve 9 and the second electric ball valve 28 are closed. The first electric push rod 19 is retracted and the second electric push rod 22 is extended.
The first syringe 20 is filled with eluent, and the tail part of the piston rod is connected with the head part of the first electric push rod 19.
The piston of the second syringe 23 is pushed to the head, and the tail of the piston rod is connected with the head of the second electric push rod 22.
And S602, collecting signals of the pressure sensor 24.
The in-situ extraction, enrichment and sampling of organic pollutants in seawater have two working modes:
one is a fixed water depth mode, and by setting the target water depth, when the signal of the pressure sensor 24 is matched with the target water depth, the extraction, enrichment and sampling work is automatically operated.
The other is a manual control mode of any water depth. By collecting the signal of the pressure sensor 24 in real time, the extraction, enrichment and sampling work is manually started on the water layer to be sampled.
And S603, opening the first electric ball valve 9, delaying for a period of time, and starting the first water pump 10.
And S604, reading signals of the first flowmeter 8 in real time, and when the volume of the sample calculated by the flowmeter reaches a preset value, closing the first water pump 10 and the first electric ball valve 9 in sequence to finish the sample introduction process.
The flow is accumulated when the step is executed each time, and the total flow is used as the calculation basis of the enrichment multiple.
And S605, closing the third electric ball valve 4 and starting the stirring motor 12 to rotate at a high speed. The nano particles are fully contacted with the seawater sample under the action of the stirring frame 13, and the extraction of the target substance is completed. And finishing stirring when the set time is counted down.
And S606, opening the third electric ball valve 4 and the second electric ball valve 28, delaying for a period of time, and starting the second water pump 29.
And S607, monitoring the second flow meter 27 in real time, and when no flow signal is output, closing the second water pump 29 and the second electric ball valve 28 in sequence to finish a drainage process.
S608, repeating S603-S607. The number of repetitions is typically determined by the level of the target substance in the sampled water area in order to obtain a suitable enriched concentration sample for subsequent monitoring analysis.
And S609, switching the multi-way valve 17 to the sample tank 1 to be communicated with the pipeline of the second injector 23. And starting the second electric push rod 22, and finishing the extraction of the water sample remained in the sample processing tank 1 by the second injector 23 under the drawing action of the push rod. The second electric putter 22 is stopped.
S610, the multi-way valve 17 is switched to the liquid discharge pipe 30 to be communicated with the pipeline of the second injector 23. The second electric push rod 22 is started, and the water sample in the second injector 23 is discharged from the liquid discharge pipe 30 under the push of the push rod, so that the water sample remained in the sample processing tank 1 is emptied. The second electric putter 22 is stopped.
S611, starting the first electric push rod 19, and injecting the eluent into the sample processing tank 1 by the first injector 20 under the push of the push rod.
Since the advancing speed of the first electric putter 19 is determined, it is only necessary to control the advancing time to control the amount of the eluent to be added. The first electric putter 19 is stopped.
And S612, closing the third electric ball valve 4 and starting the stirring motor 12 to rotate at a low speed. The nano particles are fully contacted with the eluent under the action of the screw shaft at the lower part of the stirring frame 13, and the desorption of the target substance is completed. To this end, the elution solvent contains the target substance to be measured. And waiting for the set time to count down. The time is timed to shut down the agitator motor 12.
And S613, switching the multi-way valve 17 to the sample tank to be communicated with the pipeline of the second injector 23. The second electric push rod 22 is started, and the second injector 23 finishes the extraction of the eluent in the sample processing tank 1 under the pulling action of the push rod. The second electric putter 22 is stopped.
And S614, switching the multi-way valve 17 to communicate the sampling bottle 18 with the pipeline of the second injector 23. The second electric push rod 22 is started, and the eluent in the second injector 23 enters the sampling bottle 18 under the push of the push rod, so that the target substance in the sample processing tank 1 is transferred. The second electric putter 22 is stopped.
The eluate may optionally be filled into one sample vial or may be dispensed into two sample vials for use as a replicate. And finishing the extraction, enrichment and sampling working process of the target substance.
Compared with the traditional investigation means, the extraction enrichment sampling device developed based on the invention avoids the collection, transportation and sample cross contamination of a large amount of water samples, effectively reduces the transportation and storage cost and improves the accuracy of the analysis result. The functional nano particles are adopted to replace an extraction column as an extraction medium, the extraction time is short, the efficiency is high, and the problems of extraction column blockage, fiber breakage and the like in the conventional extraction mode are avoided. The sampling process adopts a closed-open-closed mode, and the problem of cross contamination among different water layers in the submergence process of the sampling device is effectively solved. The water depth sensor is matched, so that sample collection of any target water level can be realized, the in-situ pollution condition can be truly reflected, and the seawater depth sensor is very favorable for seawater profile investigation.
Claims (10)
1. The utility model provides an organic pollutant in-situ extraction enrichment sampling device in sea water which characterized in that: the device comprises a sample extraction and enrichment unit, a sample introduction unit, a drainage unit, a pressure balance unit, a sample elution unit, a sample transfer unit and a control circuit board assembly; the sample introduction unit, the water drainage unit, the pressure balance unit, the sample elution unit and the sample transfer unit are all connected with the sample extraction and enrichment unit, and all the units are controlled by the control circuit board assembly to finish sample introduction, extraction and enrichment of organic pollutants in seawater.
2. The in-situ extraction, enrichment and sampling device for organic pollutants in seawater as claimed in claim 1, which is characterized in that: the sample extraction and enrichment unit mainly comprises a sample processing tank, a stirring motor and a stirring frame; the sample processing tank is provided with a plurality of interfaces, and the interfaces are used for connecting other units; the stirring motor is arranged on the sample processing tank through an interface and is connected with a stirring frame in the sample processing tank; the bottom end in the sample processing tank is provided with a conical closing-in; and a sample elution cavity is arranged below the conical closing-in.
3. The in-situ extraction, enrichment and sampling device for organic pollutants in seawater as claimed in claim 2, which is characterized in that: the stirring frame consists of a cylindrical sealing shaft, an annular plate type structure and a spiral shaft; the cylindrical sealing shaft is arranged at the top of the annular plate type structure, and the spiral shaft is arranged at the bottom of the annular plate type structure; the lower part of the annular plate type structure is conical and is attached to the conical closing-in of the sample processing tank.
4. The in-situ extraction, enrichment and sampling device for organic pollutants in seawater as claimed in claim 2, which is characterized in that: the sample introduction unit mainly comprises a first flowmeter, a first electric ball valve and a first water pump; the water outlet of the first water pump is connected with an interface on the sample processing tank through a pipeline; the pipeline is sequentially connected with a first electric ball valve and a first flowmeter.
5. The in-situ extraction, enrichment and sampling device for organic pollutants in seawater as claimed in claim 2, which is characterized in that: the drainage unit mainly comprises a second flowmeter, a second electric ball valve, a second water pump and a filter screen; the filter screen is arranged at the interface of the sample processing tank and is tightly attached to the interface; the second water pump is connected with the interface of the sample processing tank through a pipeline, and a second electromagnetic valve and a second flowmeter are sequentially connected to the pipeline.
6. The in-situ extraction, enrichment and sampling device for organic pollutants in seawater as claimed in claim 4 or 5, which is characterized in that: the control circuit board assembly monitors signals of the first flowmeter and the second flowmeter, and when the first flowmeter reaches a set value, the first electric ball valve and the first water pump are closed; and when the second flowmeter outputs no signal, the second electric ball valve and the second water pump are closed.
7. The in-situ extraction, enrichment and sampling device for organic pollutants in seawater as claimed in claim 2, which is characterized in that: the pressure balancing unit mainly comprises a balancing gas tank, a balancing plug and an anti-falling cover; the balance gas tank is a container with a bottom, and the bottom is provided with a vent hole; the vent hole is connected with the interface of the sample processing tank through a pipeline; the anti-drop cover is arranged at the top of the balance gas tank; the balance plug is arranged in the balance gas tank and moves up and down in the balance gas tank along with the change of external water pressure or internal air pressure.
8. The in-situ extraction, enrichment and sampling device for organic pollutants in seawater as claimed in claim 2, which is characterized in that: the sample elution unit comprises a first electric push rod, a first injector and a one-way valve; the tail part of a piston rod of the first syringe is connected with a first electric push rod; the injection end of the first injector is connected with the one-way valve through a polytetrafluoroethylene liquid pipe; the one-way valve terminal is connected with the interface of the sample processing tank through a pipeline, and the opening direction of the one-way valve points to the sample processing tank from one end of the injector; the first electric push rod is controlled by the control circuit board assembly.
9. The in-situ extraction, enrichment and sampling device for organic pollutants in seawater as claimed in claim 2, which is characterized in that: the sample transfer unit comprises an adapter, a multi-way valve, a sampling bottle, a second electric push rod and a second injector; one path of the multi-way valve is connected with an outlet of the sample elution cavity through a joint; one path is connected with the injection end of the second injector through a polytetrafluoroethylene liquid pipe, and the other path is connected with a liquid discharge pipe; at least one path is connected with a sampling bottle; the tail part of a piston rod of the second injector is connected with a second electric push rod; the second electric push rod is controlled by the control circuit board assembly.
10. An in-situ extraction, enrichment and sampling method for organic pollutants in seawater comprises the following steps:
(1) taking sufficient functionalized nano particles, and filling the sufficient functionalized nano particles into the inner cavity of the sample treatment tank in advance;
(2) injecting a seawater sample into the sample treatment tank;
(3) stirring at a high speed to ensure that the nano particles are fully contacted with the seawater sample to complete the extraction of the target substance; discharging the seawater through a drainage unit;
(4) repeating the steps (2) and (3) for multiple times to realize the enrichment of the target substance;
(5) injecting the eluent into a sample treatment tank, stirring at low speed to ensure that the nano particles are fully contacted with the eluent, and finishing desorption of the target substance;
(6) transferring the eluent obtained in the step (5) into a sample bottle through a sample transfer unit to finish sampling.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111947716A (en) * | 2020-08-12 | 2020-11-17 | 滨州学院 | Ocean vertical profile measuring device |
| CN114371048A (en) * | 2021-02-05 | 2022-04-19 | 爱威科技股份有限公司 | Sample preparation control method, control device, electronic device and sample preparation system |
-
2020
- 2020-04-08 CN CN202010267990.0A patent/CN111442966A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111947716A (en) * | 2020-08-12 | 2020-11-17 | 滨州学院 | Ocean vertical profile measuring device |
| CN114371048A (en) * | 2021-02-05 | 2022-04-19 | 爱威科技股份有限公司 | Sample preparation control method, control device, electronic device and sample preparation system |
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