CN109540641B - Device for separating and purifying microplastic in marine sediment and application method thereof - Google Patents
Device for separating and purifying microplastic in marine sediment and application method thereof Download PDFInfo
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- CN109540641B CN109540641B CN201811537368.6A CN201811537368A CN109540641B CN 109540641 B CN109540641 B CN 109540641B CN 201811537368 A CN201811537368 A CN 201811537368A CN 109540641 B CN109540641 B CN 109540641B
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- 239000013049 sediment Substances 0.000 title claims abstract description 57
- 229920000426 Microplastic Polymers 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000007788 liquid Substances 0.000 claims abstract description 63
- 239000000126 substance Substances 0.000 claims abstract description 29
- 238000007790 scraping Methods 0.000 claims abstract description 27
- 238000005192 partition Methods 0.000 claims abstract description 26
- 238000000746 purification Methods 0.000 claims description 24
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 19
- 238000000926 separation method Methods 0.000 claims description 14
- 229910052742 iron Inorganic materials 0.000 claims description 10
- 230000029087 digestion Effects 0.000 claims description 9
- 230000000694 effects Effects 0.000 claims description 9
- 239000000725 suspension Substances 0.000 claims description 8
- 239000002699 waste material Substances 0.000 claims description 8
- 208000034699 Vitreous floaters Diseases 0.000 claims description 7
- 230000009471 action Effects 0.000 claims description 7
- -1 polytetrafluoroethylene Polymers 0.000 claims description 7
- 238000001514 detection method Methods 0.000 claims description 6
- 239000003344 environmental pollutant Substances 0.000 claims description 6
- 239000000835 fiber Substances 0.000 claims description 6
- 239000012634 fragment Substances 0.000 claims description 6
- 231100000719 pollutant Toxicity 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical class [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- 238000007670 refining Methods 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 244000005700 microbiome Species 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 230000005484 gravity Effects 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 238000007605 air drying Methods 0.000 claims 1
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- 238000009434 installation Methods 0.000 abstract 1
- 238000012423 maintenance Methods 0.000 abstract 1
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- 238000000605 extraction Methods 0.000 description 6
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- 239000011148 porous material Substances 0.000 description 5
- 238000011084 recovery Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000004698 Polyethylene Substances 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- 239000004793 Polystyrene Substances 0.000 description 2
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- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 239000004800 polyvinyl chloride Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- 241000251468 Actinopterygii Species 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
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- 229920001410 Microfiber Polymers 0.000 description 1
- 238000000184 acid digestion Methods 0.000 description 1
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- 238000004458 analytical method Methods 0.000 description 1
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- 238000007796 conventional method Methods 0.000 description 1
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- 230000006862 enzymatic digestion Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 229920001684 low density polyethylene Polymers 0.000 description 1
- 239000004702 low-density polyethylene Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000003658 microfiber Substances 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
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- 239000000203 mixture Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 230000002085 persistent effect Effects 0.000 description 1
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- 229920002223 polystyrene Polymers 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 235000015170 shellfish Nutrition 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
- G01N1/38—Diluting, dispersing or mixing samples
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Biomedical Technology (AREA)
- Molecular Biology (AREA)
- Engineering & Computer Science (AREA)
- Separation Of Solids By Using Liquids Or Pneumatic Power (AREA)
- Centrifugal Separators (AREA)
Abstract
The invention discloses a device for separating and purifying microplastic in marine sediments and a use method thereof. The device consists of a separating part of the microplastic and a purifying part of the microplastic. The separating part of the micro plastic comprises a density liquid bottle, a chassis, a separable partition board, a first switch, a stirrer, a first scraping plate, a first conduit and a second switch; the top end of the density liquid bottle is provided with a branch opening; the density liquid bottle is provided with a separable baffle plate at one third of the bottom part of the density liquid bottle, and the separable baffle plate is provided with a switch, so that the baffle plate is separated from the middle, and substances such as a centrifugal device and high-density sediment sink. The bottom of the density liquid bottle is provided with a chassis and a stirrer, the scraping plate is arranged in the density liquid bottle, the bottom of the scraping plate is parallel to a branch opening at the top end of the density liquid bottle, and a first conduit with a switch is connected to the branch opening. The device has high efficiency of separating and purifying the microplastic, simple structure, easy detachment and convenient installation and maintenance.
Description
Technical Field
The invention belongs to the technical field of extraction of micro-plastics in detection sediments in marine environments, and particularly relates to a separation and purification device for micro-plastics in marine sediments and a use method thereof.
Background
The plastic is a high molecular compound prepared by taking various monomers as raw materials and adding a certain amount of additives through polymerization reaction, so that a series of characteristics such as light weight, stable chemical property, no rust and the like are generated. Currently, the production of plastic articles is very large, and related investigation shows that the production of plastic articles is doubled in the next 20 years. The recovery rate of plastic products is only about 10%, and most of the plastic products are discharged into the environment due to improper management of the rest. Because plastics are not easily degraded and have long decomposition times, a large number of plastic flakes currently exist in the environment, such as the atmosphere, sea, sediment, and the like. Differences in the composition of the plastic articles will affect their affinity for other contaminants and the potential risks associated therewith. The most common plastics in the environment are Polyethylene (PE), polyvinyl chloride (PVC), polypropylene (PP), polyethylene terephthalate (PET) and Polystyrene (PS). These waste plastic fragments are not completely degraded by exposure to sunlight, air, sea, etc., but become smaller to form microplastic with a particle size of less than 5 mm. The sizes of the microplastic are almost the same as those of fibers and plankton in the environment, and the microplastic is easy to be eaten by organisms such as shellfish, fish and the like in the environment, so that the food chain is affected. The microplastic has large surface area, is easy to combine with other pollutants in the environment to form composite pollutants, and causes persistent pollution to the environment. With development of technology and importance of people on microplastic, in particular, deep research on marine microplastic is carried out, and research work on microplastic in extraction environment is a very important link. However, the reasons of heavy equipment, high cost, poor separation effect, poor accuracy of the target object and the like are all the difficulties in extracting the microplastic in the sediment. The presently disclosed patents, such as China patent invention, grant publication number: CN 107281813A, publication date: the device is perfect, and the defects of more operation steps, low efficiency, low recovery rate and the like of other micro-plastic extraction devices are overcome, but the fibers and organisms contained in the micro-plastic cannot be subjected to evolution treatment, so that the obtained micro-plastic particles are poor in reliability, and the device is complicated. In addition, chinese patent invention, grant bulletin number: CN106769356 a, publication date: in 2017, 31, 05.h.05, a microplastic extraction device and a method thereof are disclosed, which can prevent foreign matter from interfering with extracted microplastic, but can not purify the sample itself.
In a word, since the micro-plastics have a great influence on the marine environment, the research on the development and improvement of detection technology of the related micro-plastics in the marine environment is particularly important, and the method has great significance and practical application value on the comprehensive evaluation of the marine environment.
Disclosure of Invention
The invention mainly aims to provide a separating and purifying device for microplastic of marine sediment and a using method thereof, and aims to overcome the defects of complex device for extracting microplastic in the existing sediment, poor data reliability and the like.
The technical scheme of the invention is as follows:
the device for separating and purifying the microplastic in the marine sediment consists of a separating part of the microplastic and a purifying part of the microplastic, wherein:
the separating part of the micro plastic comprises a density liquid bottle, a chassis, a separable partition board, a first switch, a stirrer, a first scraping plate, a first conduit and a second switch; the top end of the density liquid bottle is provided with a branch opening; the density liquid bottle is a bottle with the capacity of 5.0L and the diameter of 10cm, and a separable partition plate is arranged at the position, which is one third away from the bottom, of the bottle, and is provided with a switch, so that the partition plate is separated from the middle, and substances such as a centrifugal device and high-density sediment sink. The bottom of the density liquid bottle is provided with a chassis and a stirrer, the scraping plate is arranged in the density liquid bottle, the bottom of the scraping plate is parallel to a branch opening at the top end of the density liquid bottle, and the branch opening is connected with a first conduit with a switch; the method is used for separating substances such as low-density microplastic and the like in marine sediments; the outflow conduit opening of the first conduit is connected with a first-stage purifying bottle;
the purification part of the microplastic comprises a first-stage purification bottle, a second scraping plate, a switch, a second guide pipe, a second-stage purification bottle, a third scraping plate, a switch, a third guide pipe, a filter disc, a waste liquid cylinder and an iron stand table, wherein the fracture of the guide pipe is made by grinding, so that the whole system has good sealing performance. The second scraping plate or the third scraping plate is fixed and suspended at the top of the purifying bottle through an iron stand; the primary purifying bottle and the secondary purifying bottle are provided with branch ports; the primary purifying bottle is 8cm in diameter and 1.0L in capacity, and a branch port at the top end of the primary purifying bottle is connected with a second conduit with a switch; the outlet pipe orifice of the guide pipe is connected with the secondary purifying bottle; the secondary purifying bottle is 8cm in diameter and 1.0L in capacity, and a branch port at the top end of the secondary purifying bottle is connected with a third conduit with a switch; the outlet pipe orifice of the guide pipe is connected with the filter disc; the filtering disc is fixed on the iron stand, the waste liquid bottle is placed below the filtering disc, the three parts are assembled from left to right as shown in the sequence, and the outflow conduit opening of the upper stage is positioned above the container opening of the lower stage, so that the effluent of the upper stage well enters the lower stage.
Further, the density liquid bottle with the diameter of 10cm and the capacity of 5.0L is provided with a separable baffle plate with a control switch at the bottom third of the container, so that high-density and low-density objects relative to the density liquid can be fully separated.
Further, the stirrer is positioned just at the sediment so that the sediment is fully mixed with the density liquid.
Further, the filter disc is provided with gaps with the diameter of 4 meshes or 5 meshes, the filter disc is of a hollow structure, the upper layer of the filter disc is a filter sheet which is full of the gaps, and the lower layer of the filter disc is similar to a funnel device and is connected with a guide pipe.
Further, the components of the device are made of polytetrafluoroethylene materials.
The application method of the device for separating and purifying the microplastic in the marine sediment comprises the following steps:
1) Collecting 100-300 g of marine sediment, drying the sediment in an oven at 95-105 ℃, picking up massive hard substances and other substances, and refining the sediment;
2) Placing the treated marine sediment on a separable partition plate, adding 2.0-3.0L of saturated NaCl or saturated NaI density liquid, and turning on a stirrer to fully stir to form suspension; the rotating speed of the stirrer is 160-240 rpm;
3) Under the action of full stirring, the substances with low density float upwards, the substances with high density, such as sediment, sink on the partition board, the substances with high density are continuously stirred, and the separation switch of the partition board is slowly opened, so that the substances with high density sink from the separation part of the partition board due to the action of gravity, and the purpose of separating the substances with high density from the substances with low density is achieved;
4) Turning off the stirrer, standing for 10-30 minutes, turning on a switch of a right end branch port of the density liquid bottle, and enabling fragments in the upper suspension to flow into the first-stage purifying bottle from the guide pipe by using a scraper;
5) Adding biological tissue digestion liquid into a primary purification bottle, stirring by using an opening scraper to fully purify fragments in the primary purification bottle, soaking at 50-60 ℃ for 6.0-12.0 hours, removing microorganisms in marine sediments, standing for 10-30 minutes, and flowing upper-layer floaters into a secondary purification bottle from the branch port end of the primary purification bottle by using the scraper;
6) Adding acidolysis solution into a secondary purifying bottle, stirring by using an opening scraper to fully purify fragments in the secondary purifying bottle, removing fiber and partial load pollutants on the surface of microplastic in marine sediments after purifying for 6.0-12.0 hours at 30-35 ℃, and flowing upper-layer floaters into a filter disc from the branch port end of the secondary purifying bottle by using the scraper after standing for 10-30 minutes;
7) The effluent was subjected to solid-liquid separation on a filter tray and washed with deionized water, and the solids on the filter tray were collected and air-dried for detection.
In the method, the biological tissue digestion solution is an enzymolysis solution with the activity of 8.4-uhb/ml-16.8-uhb/ml.
In the method, the acidolysis solution is a dilute nitric acid solution with the mass percent concentration of 10-15%.
In the method, a separation scraper with stirring effect is arranged in the purifying bottle, and when suspected micro-plastic particles enter the purifying bottle, the stirring effect of the scraper is started to enable the purifying liquid to fully react with the suspected micro-plastic particles; when the micro plastic particles are on the surface layer of the purifying liquid, the separation effect of the scraping plate is started, so that the micro plastic on the surface layer of the solution better enters the next-stage system.
In the method, the separation part of the microplastic and the purification part of the microplastic can be used separately and independently, and can be mutually supplemented, and the microplastic extract can be further purified after being assembled together. The detachable portable bicycle is convenient to disassemble and assemble and easy to carry.
In the method, each part of the system is arranged in an opening way, so that the solution of each stage is conveniently added.
According to the method, the purifying liquid can be conveniently replaced according to the source property of the sample.
In the method, the pollutant components loaded on the surface of the microplastic can be obtained through analysis and treatment of the purifying liquid, so that the migration and conversion of pollution can be better known.
Compared with the prior art, the invention has the advantages that:
(1) All parts of the device are made of polytetrafluoroethylene materials, so that sediment is easier to suspend in a solution;
(2) In the suspension process of the sediment, the sediment is placed in the middle of a density liquid bottle, and the suspension effect of the sediment is improved under the stirring action of a stirrer, so that substances with high and low densities are fully separated;
(3) Baffle in the density liquid bottle sets up, its characteristics: the sediment is positioned in the middle of the density liquid bottle and provided with pores, and can be completely separated;
(4) The scraper with multiple functions is used, the complexity of the device is reduced firstly, the floaters can be fully digested in the purifying liquid secondly, and the floaters can be quickly flowed into a processor of the next stage thirdly;
(5) The multistage purifying bottle is arranged, so that the steps of separating, purifying and collecting microplastic in marine sediments can be continuously carried out, and impurities such as microorganisms and fibers contained in low-density matters are easily removed;
(6) The device has the advantages of continuous separation, purification and collection steps, cost saving and obvious improvement of the extraction efficiency of the microplastic.
Drawings
FIG. 1 is a schematic diagram of an extraction apparatus for microplastic in a deposit of the present invention;
FIG. 2 is a schematic diagram of a density bottle of the present invention;
FIG. 3 is a mixer retaining plate of the present invention;
FIG. 4 is a schematic view of a separable diaphragm and switch of the present invention;
FIG. 5 is a schematic view of a suspended solids flight of the present invention;
FIG. 6 is a schematic view of a filter tray of the present invention;
fig. 7 shows a support stand for a filter tray according to the present invention.
The individual components in the figure are as follows: the density liquid bottle 1, the chassis 2, the separable partition plate 3, the first switch 4, the stirrer 5, the first scraping plate 6, the first guide pipe 7, the second switch 8, the first-stage purifying bottle 9, the second scraping plate 10, the third switch 11, the second guide pipe 12 and the second-stage purifying bottle 13; a third squeegee 14; a fourth switch 15, a third conduit 16, a filter disc 17, a waste liquid tube 18 and an iron stand 19.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but embodiments of the present invention are not limited thereto, and may be performed with reference to conventional techniques for process parameters that are not specifically noted.
The device of the invention is as follows:
as shown in fig. 1 to 7, the device for separating and purifying microplastic in marine sediment is composed of a separating part of microplastic and a purifying part of microplastic, wherein: the separating part of the micro plastic comprises a density liquid bottle 1, a chassis 2 (a specific structure of a panel is provided with a fixed screw for fixing a stirrer 5, as shown in figure 2), a separable partition plate 3, a first switch 4, a stirrer 5, a first scraper 6, a first conduit 7 and a second switch 8; the top end of the density liquid bottle 1 is provided with a branch opening; the density liquid bottle 1 is a bottle with a capacity of 5.0L and a diameter of 10cm, a separable partition plate 3 is arranged at a position which is one third away from the bottom, and the separable partition plate 3 is provided with a switch 4, so that the partition plate is separated from the middle, and substances such as a centrifugal device, sediment with high density and the like sink. The bottom of the density liquid bottle 1 is provided with a chassis 2 and a stirrer 5, the scraping plate 6 is arranged in the density liquid bottle 1, the bottom of the scraping plate 6 is parallel to a branch opening at the top end of the density liquid bottle 1, and the branch opening is connected with a first conduit 7 with a switch 8; the method is used for separating substances such as low-density microplastic and the like in marine sediments; the outflow conduit opening of the first conduit 7 is connected with a primary purifying bottle 9; the purification part of the microplastic comprises a first-stage purification bottle 9, a second scraping plate 10, a switch 11, a second guide pipe 12, a second-stage purification bottle 13, a third scraping plate 14, a switch 15, a third guide pipe 16, a filter disc 17, a waste liquid cylinder 18 and an iron stand 19, wherein the fracture of the guide pipe is made by grinding, so that the whole system has good tightness. The second scraping plate 10 or the third scraping plate 14 is fixed and suspended on the top of the purifying bottle through an iron stand; the primary purifying bottle 9 and the secondary purifying bottle 13 are provided with branch ports; the primary purifying bottle 9 is 8cm in diameter and 1.0L in capacity, and a branch opening at the top end of the primary purifying bottle is connected with a second conduit 12 with a switch 11; the outflow conduit opening of the conduit 12 is connected with a secondary purifying bottle 13; the secondary purifying bottle 13 is 8cm in diameter and 1.0L in capacity, and a branch port at the top end of the secondary purifying bottle is connected with a third guide pipe 16 with a switch 15; the outflow conduit mouth of the conduit 16 is connected with a filter disc 17; the filtering tray 17 is fixed on the iron stand 19, the waste liquid bottle 18 is placed under the filtering tray, the three parts are assembled from left to right as shown in the figure, and the outflow conduit port of the upper stage is positioned above the container port of the lower stage, so that the effluent of the upper stage well enters the lower stage. The density liquid bottle 1 with the diameter of 10cm and the capacity of 5.0L is provided with a separable baffle plate 3 with a control switch 4 at the bottom third of the container, so that high-density and low-density objects relative to density liquid can be fully separated. The stirrer 5 is located just at the sediment so that the sediment is thoroughly mixed with the density liquid. The filter disc is provided with gaps, the diameter of the gaps is 4 meshes or 5 meshes, the filter disc is of a hollow structure, the upper layer of the filter disc is a filter sheet which is full of the gaps, and the lower layer of the filter disc is similar to a funnel device and is connected with a guide pipe.
The biological tissue digestion solution used in the following examples was a biological digestion enzyme solution (Shanghai Kazak Biotechnology Co., ltd.) and the acidolysis solution used was nitric acid having a concentration of 10% by mass.
Example 1
1. Collecting sediment in a sample bag at a shallow sea shore area of an environment stable zone, and carrying the sediment back to a laboratory for treatment;
2. drying the collected sediment in an oven at 95 ℃, removing massive substances, and refining;
3. preparing 3.0L of saturated sodium chloride solution, preparing biological tissue digestion solution (activity is 10 u/mL-15 u/mL), and preparing acidolysis solution such as concentrated sulfuric acid;
4. adding the refined sediment into a partition plate of the density liquid, adding the density liquid, and starting a stirrer (the rotating speed is 160 rpm) to fully stir;
5. opening a pore switch of the partition board to enable sediment to sink, standing for 30 minutes, opening a scraper to enable suspended matters to enter the branch pipe and flow into the primary purifying bottle;
6. adding the prepared enzymolysis liquid into the primary purifying bottle, starting the stirring action (the rotating speed is 80 rpm) of the scraper, fully stirring, purifying for 12 hours, enabling suspended matters to enter a branch pipe by using the scraper, and flowing into the secondary purifying bottle;
7. adding acidolysis solution into a secondary purifying bottle, starting the stirring function of a scraper (the rotating speed is 80 rpm), fully stirring, purifying for 12 hours, enabling suspended matters to enter a branch pipe by using the scraper, and flowing into a separating disc;
8. the microplastic was collected on a separation disc, air-dried, and stored for detection.
Finally, the collected micro plastic particles are subjected to infrared spectrum characterization, and all plastic products are found, wherein the main components are polystyrene and polyvinyl chloride.
Example 2
1) Collecting 500g of marine sediment, drying the marine sediment at 95 ℃, and refining the massive sediment;
2) Placing the treated sediment at a partition plate 3 in a density liquid bottle 1, adding 3.0L of saturated NaCl density liquid, and fully stirring at 160rpm to form suspension;
3) Opening a pore switch of the partition board 3 to enable pores of the partition board to sink in the high-density sediment substances, so as to separate the high-density substances from the low-density substances; the partition plate 3 can be completely opened to enable the stirrer to be arranged at the bottom of the density liquid bottle, and can be partially opened to enable sediment to sink from the pores (with the diameter of 5-10 mm);
4) Enabling the scraping plate to enable substances in the upper suspension to flow into the primary purifying bottle from the guide pipe;
5) Adding biological tissue digestion solution (activity is 10 u/mL-15 u/mL) into the primary purification bottle, enabling the biological tissue digestion solution to be subjected to full purification treatment for 12h under the stirring action of a scraper (the rotating speed is 80 rpm), standing for 30 min, and enabling the scraper to enable upper-layer floaters to flow into the secondary purification bottle from the branch port end of the primary purification bottle; the enzymolysis liquid is mainly used for digesting biological tissues;
6) Adding acidolysis solution into the secondary purifying bottle, stirring with a scraper (rotating speed is 80 rpm) to perform sufficient purifying treatment for 12h, standing for 30 min, and enabling the scraper to flow the upper layer floating matters into the filtering disc from the branch port end of the primary purifying bottle; the acidolysis solution is mainly used for removing substances such as fibers and the like, and can also lead pollutants deposited on the surface of the microplastic to fall off;
7) The effluent was subjected to solid-liquid separation on a filter tray (filter tray using a 0.45m filter membrane) and washed with deionized water, and the solids on the filter tray were collected and air-dried for detection.
Example 3
The purchased low density polyethylene particles were crushed on a crusher, 0.5234g was weighed, and 0.432g of microfiber product was added, and both were uniformly mixed with 300g of soil as a simulated sediment sample.
The primary enzymatic digestion step was removed and the acid digestion was performed directly, with other procedures consistent with example 1.
And finally, drying the obtained micro plastic particles on the filter disc, and preserving and detecting the micro plastic particles. The recovery rate of the sample reaches 97.6%, and the micro particles are detected by infrared spectrum, and all the samples are microplastic.
Claims (1)
1. The device for separating and purifying the microplastic in the marine sediment is characterized by comprising a separating part of the microplastic and a purifying part of the microplastic, wherein:
the separating part of the micro plastic comprises a density liquid bottle (1), a chassis (2), a separable partition board (3), a first switch (4), a stirrer (5), a first scraper (6), a first conduit (7) and a second switch (8); the top end of the density liquid bottle (1) is provided with a branch opening; a separable partition plate (3) is arranged at one third of the density liquid bottle (1) away from the bottom, the separable partition plate (3) is provided with a first switch (4), the bottom of the density liquid bottle (1) is provided with a chassis (2) and a stirrer (5), the first scraping plate (6) is arranged in the density liquid bottle (1), the bottom of the first scraping plate (6) is parallel to a branch opening at the top end of the density liquid bottle (1), and the branch opening is connected with a first guide pipe (7) with a second switch (8); the outflow conduit opening of the first conduit (7) is connected with a first-stage purifying bottle (9);
the purification part of the micro plastic comprises a first-stage purification bottle (9), a second scraping plate (10), a third switch (11), a second guide pipe (12), a second-stage purification bottle (13), a third scraping plate (14), a fourth switch (15), a third guide pipe (16), a filter disc (17), a waste liquid barrel (18) and an iron stand (19); the second scraping plate (10) or the third scraping plate (14) is fixed and suspended at the top of the purifying bottle through an iron stand; the primary purifying bottle (9) and the secondary purifying bottle (13) are provided with branch ports; the branch opening at the top end of the primary purifying bottle (9) is connected with a second conduit (12) with a third switch (11); the outlet pipe mouth of the second conduit (12) is connected with a secondary purifying bottle (13); the branch opening at the top end of the secondary purifying bottle (13) is connected with a third conduit (16) with a fourth switch (15); the outlet pipe mouth of the third pipe (16) is connected with a filter disc (17); the filter disc (17) is fixed on the iron stand (19), and a waste liquid cylinder (18) is arranged below the filter disc;
the stirrer (5) is positioned at the position just at the sediment so that the sediment and the density liquid are fully mixed;
the filter disc is provided with gaps with the diameter of 4 meshes or 5 meshes, the filter disc is of a hollow structure, the upper layer of the filter disc is a filter sheet which is full of the gaps, and the lower layer of the filter disc is similar to a funnel device and is connected with a guide pipe;
parts of the device are made of polytetrafluoroethylene materials;
the application method of the device for separating and purifying the microplastic in the marine sediment comprises the following steps:
1) Collecting 100-300 g of marine sediment, drying the sediment in an oven at 95-105 ℃, picking out massive hard substances and other substances, and refining the sediment;
2) Placing the treated marine sediment on a separable partition plate, adding 2.0-3.0L of saturated NaCl or saturated NaI density liquid, and turning on a stirrer to fully stir to form suspension; the rotational speed of the stirrer is 160-240 rpm;
3) Under the action of full stirring, the substances with low density float upwards, the substances with high density, such as sediment, sink on the partition board, the substances with high density are continuously stirred, and the separation switch of the partition board is slowly opened, so that the substances with high density sink from the separation part of the partition board due to the action of gravity, and the purpose of separating the substances with high density from the substances with low density is achieved;
4) Turning off the stirrer, standing for 10-30 min, turning on the switch of the right branch port of the density liquid bottle, and enabling the debris in the upper suspension to flow into the first-stage purifying bottle from the guide pipe by using the scraping plate;
5) Adding biological tissue digestion solution into the primary purification bottle, stirring by using an opening scraper to fully purify fragments in the primary purification bottle, soaking at 50-60 ℃ for 6.0-12.0 hours, removing microorganisms in marine sediments, standing for 10-30 minutes, and flowing upper-layer floaters into the secondary purification bottle from the branch port end of the primary purification bottle by using the scraper;
6) Adding acidolysis solution into a secondary purifying bottle, stirring by using an opening scraper to fully purify fragments in the secondary purifying bottle, removing fiber and partial load pollutants on the surface of microplastic in marine sediments after purifying for 6.0-12.0 hours at 30-35 ℃, and flowing upper-layer floaters into a filter disc from the branch port end of the secondary purifying bottle by using the scraper after standing for 10-30 minutes;
7) Performing solid-liquid separation on the effluent on a filter disc, cleaning with deionized water, and collecting and air-drying the solid on the filter disc for detection;
the biological tissue digestion solution is an enzymolysis solution with the activity of 8.4u/ml-16.8 u/ml;
the acidolysis solution is a dilute nitric acid solution with the mass percentage concentration of 10-15%.
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| CN111346729A (en) * | 2020-03-10 | 2020-06-30 | 天津市生态环境监测中心 | High-efficiency separation device and separation method for marine micro-plastic |
| JP7452655B2 (en) * | 2020-06-29 | 2024-03-19 | 株式会社島津製作所 | Sample purification equipment, analysis system |
| JP7548310B2 (en) * | 2020-06-29 | 2024-09-10 | 株式会社島津製作所 | Sample purification device, analysis system, sample purification method, and control program |
| CN112642592A (en) * | 2020-12-02 | 2021-04-13 | 苏州海狸生物医学工程有限公司 | Flotation device for micron-sized materials |
| CN118541218A (en) * | 2021-12-28 | 2024-08-23 | 株式会社岛津制作所 | Purification device and control method for purification device |
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