CN113834716A - Continuous separation device for micro-plastics with different densities and application thereof - Google Patents

Continuous separation device for micro-plastics with different densities and application thereof Download PDF

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CN113834716A
CN113834716A CN202111022142.4A CN202111022142A CN113834716A CN 113834716 A CN113834716 A CN 113834716A CN 202111022142 A CN202111022142 A CN 202111022142A CN 113834716 A CN113834716 A CN 113834716A
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plastics
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CN113834716B (en
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刘禹
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Inner Mongolia Agricultural University
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    • G—PHYSICS
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    • G01N1/00—Sampling; Preparing specimens for investigation
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    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
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    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G01N1/4077—Concentrating samples by other techniques involving separation of suspended solids
    • G01N2001/4088—Concentrating samples by other techniques involving separation of suspended solids filtration
    • G—PHYSICS
    • G01—MEASURING; TESTING
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    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
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    • G01N2015/1024—Counting particles by non-optical means
    • G—PHYSICS
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    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
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    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract

The invention relates to the field of water environment protection, in particular to a continuous separation device for micro-plastics with different densities and application thereof. The device comprises a separation pipeline and a return pipeline; the upper end of the separation pipeline is provided with a sample inlet, and the lower end of the separation pipeline is provided with a high-pressure gas inlet; a first rotary spray head, a reversible screen, a first valve, a second rotary spray head, a second valve and a third rotary spray head are sequentially arranged in a pipeline between the sample inlet and the high-pressure gas inlet from top to bottom; the rotary spray head is externally connected with a high-pressure fluid infusion flusher; a waste liquid pipe is arranged on a pipeline between the reversible screen and the first valve, and a third valve is arranged in the waste liquid pipe; an overflow pipe is arranged on a pipeline between the second rotary spray nozzle and the second valve; an opening at the upper end of the return pipeline is arranged on a pipeline between the sample inlet and the first rotary spray head; the lower end of the return pipeline is communicated with the lower end of the separation pipeline; the high-pressure gas inlet faces the return pipeline and is externally connected with a high-pressure gas pump. The device can efficiently and accurately separate micro-plastics with different densities in a water sample.

Description

Continuous separation device for micro-plastics with different densities and application thereof
Technical Field
The invention relates to the field of water environment protection, in particular to a continuous separation device for micro-plastics with different densities and application thereof.
Background
The plastic has the characteristics of low price, no rustiness, no decay, low quality, good insulating property and the like, and is widely used in various aspects of human life. According to statistics, the total production amount of the global plastic reaches 3.48 hundred million tons in 2017, and the increase of 330 hundred million tons of plastic products is expected to be realized by 2050. However, only a small portion of the waste plastics can be recycled or incinerated, and most of the waste plastics are buried deeply in landfills or accumulated in the natural environment. Waste plastics in the environment degrade extremely slowly, but under some physical and chemical actions, large garbage can form plastic scraps, and when the diameter of the scraps is less than 5mm, the scraps can be defined as Micro Plastics (MPs). Human daily life can also directly generate a large amount of micro-plastics, for example, in the process of washing clothes, nearly 2000 fiber particles can be generated in each washing and enter domestic sewage, and the concentration of the micro-plastics in the sewage can reach 100 per liter; particulate additives, detergents and various industrial materials in cleaning products all contain a large amount of micro-plastics. Due to the wide use of plastic products and the multi-path source of micro-plastics, the plastic products are widely available in natural water body environments such as oceans, lakes, rivers, reservoirs and the like.
The micro plastic can cause a series of negative effects after entering the water environment. For example, micro-plastics are easily eaten by plankton, fish, and other organisms in the water. Toxicity investigation on the micro-plastics shows that the micro-plastic particles have certain harm to various aquatic organisms, such as inhibiting the growth of phytoplankton, influencing the ingestion and the movement capability of zooplankton, harming the filter feeding behavior and the reproduction of oysters, causing diseases of fishes, and the like; the micro plastic has small size, large specific surface area and strong hydrophobicity, and is a carrier for heavy metals and pollutants such as organic matter cyclic aromatic hydrocarbons (PAHs), polybrominated diphenyl ethers (PBDEs) and the like. In addition, the microplastics also contain many chemical additives, such as stabilizers, plasticizers, flame retardants or antioxidants, which are harmful to the environment, are usually added during the production process in order to improve the properties of the plastic or to prolong its lifetime.
Common micro-plastics in water environment mainly comprise Polyethylene (PE), polypropylene (PP), Polyamide (PA), Polystyrene (PS), polyvinyl chloride (PVC), polyethylene terephthalate (PET), Polyester (Polyester) and the like, and the influence of different components of the micro-plastics on the water environment is different. Therefore, when the pollution of the micro-plastic in the water environment is explored, the components of the micro-plastic need to be identified. At present, the more common identification methods include fourier transform infrared spectroscopy, raman spectroscopy, thermal analysis, mass spectrometry, scanning electron microscopy, and the like. Although the method has the advantages of high identification accuracy, no destructiveness, low sample quantity test, high throughput screening and environmental friendliness, the detection cost is high, the time is long, only a small amount of randomly selected micro-plastics can be detected, and the representativeness of the detection result is not high.
The densities of different types of micro-plastics are different, so the density separation method is an effective means for identifying the micro-plastics in the water environment. And the types of the micro-plastics in a single lake, river or reservoir generally do not exceed 7-8, and the determination of the components of the micro-plastics can be completely realized by a density separation method. However, the existing micro-plastic density separation method can only identify micro-plastic in one density range (for example, less than 1.2 g/cm)3Or less than 1.4g/cm3) This may include a plurality of types of micro-plastics, which have low precision and low overall efficiency, and thus the types of micro-plastics cannot be accurately determined. Therefore, a technology for separating the micro-plastics efficiently based on density separation is urgently needed so as to comprehensively determine the abundance and the proportion of the micro-plastics with different components.
Disclosure of Invention
In order to meet the requirements of the field, the invention provides a micro-plastic continuous separation device and method based on density separation, which realize the integrated operation of filtering, washing an instrument and overflowing in the separation process of micro-plastics with different densities, can efficiently and accurately separate the micro-plastics with different densities in a water body, can be used for measuring the number of the micro-plastics with different densities in the water body, and can determine the abundance and proportion of the micro-plastics with different components in the water body.
On one hand, the invention provides a continuous separation device for micro-plastics with different densities, which is characterized by comprising a separation pipeline and a return pipeline which are communicated with each other in a gas-liquid manner;
the upper end of the separation pipeline is provided with a sample inlet 1, and the lower end of the separation pipeline is provided with a high-pressure gas inlet 2; a first rotary nozzle 3, a reversible screen 4, a first valve 5, a second rotary nozzle 6, a second valve 7 and a third rotary nozzle 8 are sequentially arranged in a pipeline between the sample inlet 1 and the high-pressure gas inlet 2 from top to bottom;
wherein the first rotating nozzle 3, the second rotating nozzle 6 and the third rotating nozzle 8 are externally connected with a high-pressure fluid infusion flusher 9; a waste liquid outlet 10 is arranged on a pipeline between the reversible screen 4 and the first valve 5, the waste liquid outlet 10 is externally connected with a waste liquid pipe 11, and a third valve 12 is arranged in the waste liquid pipe 11; an overflow port 13 is arranged on a pipeline between the second rotary spray head 6 and the second valve 7, and the overflow port 13 is externally connected with an overflow pipe 14;
an opening at the upper end of the return pipeline is arranged on a pipeline between the sample inlet 1 and the first rotary spray head 3; the lower end of the return pipeline is communicated with the lower end of the separation pipeline; the high-pressure air inlet 2 faces the return pipeline and is externally connected with a high-pressure air pump 15.
Preferably, the pipeline between the second rotary sprayer 6 and the overflow port 13 is disconnected, and a conical funnel 16 is arranged at the disconnected part; the opening at the upper end of the funnel body of the conical funnel 16 is right opposite to the pipe orifice below the second rotary spray head 6, and the lower end of the neck of the conical funnel 16 extends into the pipe orifice above the overflow port 13.
Preferably, the conduit between the overflow 13 and the second valve 7, close to the second valve 7, is expanded in a spherical shape.
Preferably, the continuous separation device further comprises a waste liquid cylinder 17 and a liquid storage bottle 18; the outlet of the waste liquid pipe 11 leads to a waste liquid cylinder 17; the outlet of the overflow tube 14 leads to a reservoir 18.
Preferably, the continuous separation device further comprises a water bath constant temperature oscillator 19 and a vacuum filtration device 20.
Preferably, the pipes of the separation line and the return line are made of stable glass.
In another aspect, the invention provides a method for separating micro plastics with different densities in a sample, which is characterized in that any one of the continuous separation devices is used for separating the micro plastics with different densities in a water sample.
Preferably, the separation method comprises the steps of:
s1, closing a first valve 5 and a second valve 7, and opening a third valve 12; adding a water sample to be detected into a sample inlet 1, enabling the liquid to flow downwards and be filtered by a reversible screen 4, intercepting micro plastic in the liquid by the reversible screen 4, and discharging filtrate through a waste liquid pipe 11;
s2, closing the second valve 7 and the third valve 12, and opening the first valve 5; turning over the reversible screen 4 to make the surface of the screen loaded with the micro-plastics face downwards;
s3, adding a first solution into the high-pressure fluid infusion flusher 9 to enable the opening of the first rotary spray head 3 to face downwards and the opening of the second rotary spray head 6 to face upwards, then alternately using the first rotary spray head 3 and the second rotary spray head 6 to flush the reversible screen 4, and completely flushing the entrapped micro-plastic;
s4, standing to enable the micro plastic with the density larger than that of the first solution to be precipitated; the second rotary spray head 6 is opened to supplement the first solution into the pipeline, so that the micro plastic with the density smaller than that of the first solution flows into the liquid storage bottle 18 through the overflow port 13;
s5, closing the first valve 5, and opening the second valve 7 and the third valve 12; starting the high-pressure air pump 15, pressing the residual liquid in the separation pipeline into the return pipeline through high-pressure air, and making the residual liquid flow back to the upper end of the separation pipeline; the residual liquid is filtered by the reversible screen 4, the residual micro-plastic is intercepted by the reversible screen 4, and the filtrate is discharged through the waste liquid pipe 11;
s6, replacing the first solution in the high-pressure fluid infusion flusher 9 with a second solution with higher density, and repeating the steps S2-S5 to collect the micro plastic with the density higher than that of the first solution and lower than that of the second solution; and the operation is carried out until micro plastics in various density ranges in the water sample are collected.
Preferably, the separation method further comprises the steps of:
and S7, starting a water bath constant temperature oscillator 19, fully oscillating the micro plastic suspension in each liquid storage bottle 18, respectively pumping and filtering the micro plastic in each density range to a filter membrane by using a vacuum pumping and filtering device 20 after oscillation is finished, putting the filter membrane into a glass culture dish, and air-drying at room temperature to be detected.
In yet another aspect, the present invention provides a method for determining the abundance of a micro-plastic in a sample, characterized in that the method of the present invention is used to separate micro-plastics of different densities in the sample, and then the micro-plastics of different densities are subjected to component identification and enumeration.
Has the advantages that: the continuous separation device provided by the invention realizes the integrated operation of filtering, flushing, overflowing and refluxing in the separation process of the micro-plastics with different densities, can efficiently and accurately separate the micro-plastics with different densities in a water sample, and greatly shortens the manual operation time. The device has certain connectivity and leakproofness, and is provided with the high-pressure fluid infusion flusher and the high-pressure air pump, so that the loss and the residue of the micro-plastic in the experimental process are avoided, the defects of complex operation, large error and low efficiency in the existing micro-plastic separation technology are overcome, and the familiar separation of the micro-plastic in the water sample is greatly ensured. The device of the invention is adopted to separate the micro-plastics with different densities in the sample and carry out component identification and counting on the micro-plastics with different density ranges, so that the number of the micro-plastics with different densities in the sample, and the abundance and proportion of the micro-plastics with different components can be obtained.
Drawings
FIG. 1 is a schematic diagram of a continuous separation apparatus for microplastics of different densities in an exemplary embodiment of the invention; the arrows in the figure indicate the direction of liquid flow.
FIG. 2 is a schematic diagram of a continuous separation apparatus for microplastics of different densities in another exemplary embodiment of the invention; the arrows in the figure indicate the direction of liquid flow.
Fig. 3 is a schematic structural diagram of a continuous separation device for micro-plastics with different densities in another exemplary embodiment of the invention.
FIG. 4. abundance of various micro-plastics in water samples of Umbilism sea.
FIG. 5 shows the Fourier transform infrared spectrum detection result of polyethylene.
FIG. 6 shows the Fourier transform infrared spectrum detection result of polystyrene.
FIG. 7 shows the Fourier transform infrared spectrum detection result of polybutylene terephthalate.
Reference numerals: 1-sample inlet, 2-high pressure gas inlet, 3-first rotary spray head, 4-reversible screen, 5-first valve, 6-second rotary spray head, 7-second valve, 8-third rotary spray head, 9-high pressure fluid infusion flusher, 10-waste liquid outlet, 11-waste liquid pipe, 12-third valve, 13-overflow port, 14-overflow pipe, 15-high pressure air pump, 16-conical funnel, 17-waste liquid cylinder, 18-liquid storage bottle, 19-water bath constant temperature oscillator, 20-vacuum filtration device, 21-microscope, 22-linkage switch.
Detailed Description
The technical scheme of the invention is clearly and completely described below by combining the drawings and the specific embodiment.
As shown in FIG. 1, the invention provides a continuous separation device for micro-plastics with different densities, which is characterized by comprising a separation pipeline and a return pipeline which are communicated with each other in a gas-liquid manner;
the upper end of the separation pipeline is provided with a sample inlet 1, and the lower end of the separation pipeline is provided with a high-pressure gas inlet 2; a first rotary nozzle 3, a reversible screen 4, a first valve 5, a second rotary nozzle 6, a second valve 7 and a third rotary nozzle 8 are sequentially arranged in a pipeline between the sample inlet 1 and the high-pressure gas inlet 2 from top to bottom;
wherein the first rotating nozzle 3, the second rotating nozzle 6 and the third rotating nozzle 8 are externally connected with a high-pressure fluid infusion flusher 9; a waste liquid outlet 10 is arranged on a pipeline between the reversible screen 4 and the first valve 5, the waste liquid outlet 10 is externally connected with a waste liquid pipe 11, and a third valve 12 is arranged in the waste liquid pipe 11; an overflow port 13 is arranged on a pipeline between the second rotary spray head 6 and the second valve 7, and the overflow port 13 is externally connected with an overflow pipe 14;
an opening at the upper end of the return pipeline is arranged on a pipeline between the sample inlet 1 and the first rotary spray head 3; the lower end of the return pipeline is communicated with the lower end of the separation pipeline; the high-pressure air inlet 2 faces the return pipeline and is externally connected with a high-pressure air pump 15.
In the continuous separation device of the invention, the used rotary spray head is a spray head which can change the direction of the spray head so as to change the liquid spraying direction; the opening and closing, the direction and the liquid spraying speed of the first rotary sprayer 3, the second rotary sprayer 6 and the third rotary sprayer 8 are all controlled by a high-pressure liquid supplementing flusher 9; the high-pressure fluid infusion irrigator 9 is also called a "high-pressure fluid infusion" or "high-pressure irrigator"; the invertible screen 4 used is a screen whose mesh surface can be inverted so as to change the mesh surface orientation; the size of the reversible screen 4 is exactly matched with the size of the inside of the pipeline of the separation pipeline, so that all water samples are filtered by the reversible screen 4; the first valve 5, the second valve 7 and the third valve 12 are pipeline fluid switches and are used for controlling the flow of liquid in a pipeline; the overflow opening 13, the overflow pipe 14, the second valve 7 and the conduit between the overflow opening 13 and the second valve 7 together constitute an overflow construction. The invention realizes the continuous separation of different-density micro-plastics in the same sample by the ingenious design and combination of the reversible screen, the three valves, the three rotary nozzles, the overflow structure and the application of the return pipeline. The sample can be a directly collected water sample or a water sample obtained after collected sediments are treated.
The working process of the continuous separation device is as follows:
(1) and (3) interception: closing the first valve 5 and the second valve 7, and opening the third valve 12; the collected water sample is injected into the separation pipeline through the sample inlet 1, the liquid flows downwards, and after being filtered by the reversible screen 4, the micro plastic is intercepted on the reversible screen 4.
(2) Washing: closing the second valve 7 and the third valve 12, and opening the first valve 5; turning the reversible screen 4 by 180 degrees to make the surface loaded with the micro-plastic face downwards; and adding a first solution into a high-pressure fluid infusion flusher 9, enabling the opening of the first rotary spray head 3 to face downwards and the opening of the second rotary spray head 6 to face upwards, and alternately using the first rotary spray head 3 and the second rotary spray head 6 to flush the screen mesh from the upper part and the lower part of the reversible screen mesh 4 respectively until all the micro-plastics on the screen mesh are flushed.
(3) Standing: the first and second rotary nozzles 3 and 6 are closed, and the apparatus is left standing for a period of time (e.g., 6 hours or more) to allow the micro plastic in the mixed solution with a density greater than that of the first solution to be sufficiently precipitated into the pipe above the second valve (i.e., the bottom of the overflow structure), while the micro plastic with a density less than that of the first solution is suspended in the first solution.
(4) Overflowing: after the standing is finished, the second rotary spray head 6 is opened, the first solution is supplemented into the pipeline, and when the liquid level is higher than the position of the overflow port 13, the liquid flows into the first liquid storage bottle through the overflow pipe 14. The operations of standing and overflowing are repeated three times, and all the micro-plastic with the density lower than that of the first solution in the water sample can be collected basically.
(5) Refluxing: after the third overflow operation is finished, closing the first valve 5, opening the second valve 7 and the third valve 12, and starting the high-pressure air pump 15; at this time, the residual liquid in the separation pipeline flows downwards, and flows into the starting end of the separation pipeline again through the return pipeline under the action of high-pressure gas provided by the high-pressure gas pump 15; after the liquid is filtered by the reversible screen 4, the micro plastic with the density larger than that of the first solution is trapped on the screen, and the filtered first solution is discharged through a waste liquid pipe 11.
(6) And (3) replacing the first solution in the high-pressure fluid infusion flusher 9 with a second solution with higher density, repeating the operations (2) to (5), collecting all the micro-plastics with the density higher than that of the first solution and lower than that of the second solution in the water sample, and filling the micro-plastics into a second liquid storage bottle. The separation is continued in this way until all the microplastics of the respective density range have been collected.
In some embodiments, the corresponding solution is used to flush the pipe between the second valve 7 and the high pressure gas inlet 2 through the third rotary spray head 8, avoiding the residue of micro-plastic, thereby increasing the micro-plastic collection rate.
In some embodiments, the conduit between the second rotary sprayer 6 and the overflow 13 is interrupted, where a conical funnel 16 is provided; the opening at the upper end of the funnel body of the conical funnel 16 is right opposite to the pipe orifice below the second rotary spray head 6, and the lower end of the neck of the conical funnel 16 extends into the pipe orifice above the overflow port 13. The use of the conical hopper 16 makes it possible to slow down the flow rate of the liquid coming out from the second rotary sprayer 6, avoiding the newly added liquid from disturbing the micro-plastics previously deposited in the pipe above the second valve 7, thus improving the precision of the separation of the micro-plastics of different densities.
In some embodiments, the conduit between the overflow 13 and the second valve 7, and adjacent to the second valve 7, is bulbous. The overflow structure is similar to a round bottom overflow flask which is common in laboratories, and is beneficial to the separation of micro-plastics with different densities.
In some embodiments, the continuous separation apparatus further comprises a waste liquid tank 17; the outlet of the waste pipe 11 opens into a waste tank 17.
In some embodiments, the continuous separation apparatus further comprises a reservoir 18; the outlet of the overflow tube 14 leads to a reservoir 18. The liquid storage bottle 18 is used for collecting micro-plastic suspension, and micro-plastics with different densities are collected into different liquid storage bottles 18.
In some embodiments, the reservoir 18 is a conical flask.
In some embodiments, the continuous separation device further comprises a water bath constant temperature oscillator 19 and a vacuum filtration device 20.
In some embodiments, the vacuum filtration device 20 is a vacuum filtration device conventional in the art, including a vacuum filtration pump, a filter bowl, a filter flask, and a filter membrane.
In some embodiments, the vacuum filtration of the microplastic is carried out using a filter membrane having a pore size of 0.7 μm.
In some embodiments, the conduits of the separation line and the return line are made of stabilized glass. The stable glass is structurally stable glass, has a regular molecular structure, and has a hard glass surface.
In some embodiments, the pipe corner of the micro-plastic separation loop adopts an arc design, so that micro-plastic residues in the pipe are avoided, and the accuracy of the micro-plastic abundance measurement is improved.
In some embodiments, the invertible screen 4 is made of stainless steel.
In some embodiments, the invertible screen 4 is capable of retaining all particle sizes of micro-plastics in a sample of water.
In other embodiments, the invertible screen 4 with a desired aperture is made to retain micro-plastics with a desired particle size.
In some embodiments, the invertible screen 4 has a mesh opening size of 50 μm.
In some embodiments, the first valve 5 is close to the lower edge of the waste liquid outlet 10, so as to reduce the waste liquid residue in the pipeline above the first valve 5 as much as possible, avoid the waste liquid from polluting or diluting the solution for separating the micro-plastics with different densities, and improve the separation precision.
In some embodiments, the first valve 5, the second valve 7, and the third valve 12 are all rotatable glass valves.
In some embodiments, the high-pressure fluid replacement flusher 9 includes a high-pressure pump, a reservoir, a pressure gauge, and a gang switch 22; a liquid inlet of the high-pressure pump is connected with a liquid storage bottle through a liquid inlet pipe, and a liquid outlet of the high-pressure pump is respectively connected with the first rotary sprayer 3, the second rotary sprayer 6 and the third rotary sprayer 8 through a liquid outlet pipe; the linkage switch 22 is used for controlling the opening and closing and the orientation of the rotary spray head and the opening and closing of the high-pressure pump; the high-pressure pump is turned on at the same time as the rotary sprayer is turned on using the gang switch 22.
The invention also provides a method for separating the micro-plastics with different densities in the sample, which is characterized in that any one of the continuous separation devices is used for separating the micro-plastics with different densities in the water sample.
In some embodiments, the sample is a water sample collected directly from the environment.
In other embodiments, the sample is a sample obtained by treating the collected sediment, for example, by resuspending the sediment with distilled water, filtering to remove large-particle impurities from the suspension, and precipitating to remove silt.
In some embodiments, the separation method comprises the steps of:
s1, closing a first valve 5 and a second valve 7, and opening a third valve 12; adding a water sample to be detected into a sample inlet 1, enabling the liquid to flow downwards and be filtered by a reversible screen 4, intercepting micro plastic in the liquid by the reversible screen 4, and discharging filtrate through a waste liquid pipe 11;
s2, closing the second valve 7 and the third valve 12, and opening the first valve 5; turning over the reversible screen 4 to make the surface of the screen loaded with the micro-plastics face downwards;
s3, adding a first solution into the high-pressure fluid infusion flusher 9 to enable the opening of the first rotary spray head 3 to face downwards and the opening of the second rotary spray head 6 to face upwards, then alternately using the first rotary spray head 3 and the second rotary spray head 6 to flush the reversible screen 4, and completely flushing the entrapped micro-plastic;
s4, standing to enable the micro plastic with the density larger than that of the first solution to be precipitated; the second rotary spray head 6 is opened to supplement the first solution into the pipeline, so that the micro plastic with the density smaller than that of the first solution flows into the liquid storage bottle 18 through the overflow port 13;
s5, closing the first valve 5, and opening the second valve 7 and the third valve 12; starting the high-pressure air pump 15, pressing the residual liquid in the separation pipeline into the return pipeline through high-pressure air, and making the residual liquid flow back to the upper end of the separation pipeline; the residual liquid is filtered by the reversible screen 4, the residual micro-plastic is intercepted by the reversible screen 4, and the filtrate is discharged through the waste liquid pipe 11;
s6, replacing the first solution in the high-pressure fluid infusion flusher 9 with a second solution with higher density, and repeating the steps S2-S5 to collect the micro plastic with the density higher than that of the first solution and lower than that of the second solution; and the operation is carried out until micro plastics in various density ranges in the water sample are collected.
In some embodiments, the separation method further comprises the steps of:
and S7, starting a water bath constant temperature oscillator 19, fully oscillating the micro plastic suspension in each liquid storage bottle 18, respectively pumping and filtering the micro plastic in each density range to a filter membrane by using a vacuum pumping and filtering device 20 after oscillation is finished, putting the filter membrane into a glass culture dish, and air-drying at room temperature to be detected.
In some embodiments, the liquid storage bottles 18 containing the micro-plastics with different densities are placed in a water bath constant temperature oscillator 19 at 25-90 ℃ and oscillated at 40-80 rpm for 12-24 hours to remove impurities, so as to reduce the background value of the micro-plastics observed under a microscope.
In some embodiments, step S5 of the separation method further includes: and a corresponding solution is used for flushing a pipeline between the second valve 7 and the high-pressure gas inlet 2 through the third rotary spray head 8, so that the residue of the micro-plastic is avoided, and the micro-plastic collection rate is improved.
The invention also provides a method for measuring the abundance of the micro-plastics in the sample, which is characterized in that the method is used for separating the micro-plastics with different densities in the sample, and then carrying out component identification and counting on the micro-plastics with different densities.
In some embodiments, the micro-plastics are identified in composition using the microscope 21 and the component micro-plastics are counted using the counting software.
In some embodiments, the microscope 21 is a body microscope.
Examples of the experiments
To verify the separation effect of the continuous separation device for micro-plastics with different densities, provided by the invention, four kinds of micro-plastics with known components (detected by Fourier infrared spectroscopy) are selected firstly, and the four kinds of micro-plastics are artificial fibers (1.48 g/cm)3) Polyester (density 1.38 g/cm)3) Polystyrene (1.05 g/cm)3) And polyethylene (0.96 g/cm)3) 20 in number, 0.5mm-5mm in size, and in the shape of fiber, chip, and film. All the four types of micro-plastics are mixed into 1L of distilled water to be used as a water sample to be detected.
Then preparing solutions with different densities: the density was 1.0g/cm3Distilled water (denoted as X1 solution) having a density of 1.2g/cm3Is a saturated sodium chloride solution (denoted as X2 solution) having a density of 1.3g/cm3The potassium formate solution (designated as X3 solution) had a density of 1.4g/cm3The potassium formate solution (referred to as X4 solution) of (1). And then separating the micro-plastics with different densities in the water sample to be detected by adopting the continuous separation device.
The structure of the continuous separation device is shown in fig. 3 and comprises a micro-plastic separation loop; the micro-plastic separation loop consists of a separation pipeline and a return pipeline which are communicated with each other in a gas-liquid manner; the upper end of the separation pipeline is provided with a sample inlet 1, and the lower end of the separation pipeline is provided with a high-pressure gas inlet 2; a first rotary nozzle 3, a reversible screen 4, a first valve 5, a second rotary nozzle 6, a second valve 7 and a third rotary nozzle 8 are sequentially arranged in a pipeline between the sample inlet 1 and the high-pressure gas inlet 2 from top to bottom; the first rotating nozzle 3, the second rotating nozzle 6 and the third rotating nozzle 8 are respectively externally connected with a high-pressure fluid infusion flusher 9; a waste liquid outlet 10 is arranged on a pipeline between the reversible screen 4 and the first valve 5, the waste liquid outlet 10 is externally connected with a waste liquid pipe 11, a third valve 12 is arranged in the waste liquid pipe 11, and a water outlet of the waste liquid pipe 11 leads to a waste liquid cylinder 17; an overflow port 13 is arranged on a pipeline between the second rotary sprayer 6 and the second valve 7, the overflow port 13 is externally connected with an overflow pipe 14, and a water outlet of the overflow pipe 14 leads to a liquid storage bottle 18; the pipeline between the second rotary spray head 6 and the overflow port 13 is disconnected, and a conical funnel 16 is arranged at the disconnected position; an opening at the upper end of the funnel body of the conical funnel 16 is over against a pipe orifice below the second rotary spray head 6, and the lower end of the neck of the conical funnel 16 extends into the pipe orifice above the overflow port 13; the pipeline between the overflow port 13 and the second valve 7 and close to the second valve 7 is expanded to be spherical (similar to a round bottom overflow flask commonly used in laboratories, and for convenience of description, the structure is simply referred to as an overflow flask in the following experiments); an opening at the upper end of the return pipeline is arranged on a pipeline between the sample inlet 1 and the first rotary spray head 3; the lower end of the return pipeline is communicated with the lower end of the separation pipeline; the high-pressure air inlet 2 faces the return pipeline and is externally connected with a high-pressure air pump 15; the pipes of the separation pipe and the return pipe are made of stable glass.
The separation process of the micro-plastics with different densities comprises the following steps:
1. first, the first valve 5 and the second valve 7 are kept closed, and the third valve 12 is opened. The prepared water sample is added into the separation pipeline through the sample inlet 1, after being filtered by the reversible screen 4, all the micro-plastics in the water sample are intercepted by the reversible screen 4, and all the filtrate flows into the waste liquid cylinder 17 through the waste liquid pipe 11.
2. The second valve 7 and the third valve 12 are closed and the first valve 5 is opened. The invertible screen 4 is inverted so that the surface of the microplastic-laden web faces downward.
3. Adding X1 solution into the high-pressure fluid infusion flusher 9, twisting the spray head (second rotary spray head 6) in the middle of the high-pressure fluid infusion flusher 9 upwards, and then sequentially and repeatedly starting the spray head (first rotary spray head 3) at the top of the high-pressure fluid infusion flusher 9 and the spray head (second rotary spray head 6) in the middle to simultaneously wash the upper surface and the lower surface of the reversible screen 4, so that the micro plastic on the screen surface can be more easily washed off. The entire amount of material filtered on invertible screen 4 was flushed into the overflow flask.
4. Standing for 6 hours. Then a spray head (a second rotary spray head 6) at the middle part of the high-pressure liquid supplementing flusher 9 is opened, the X1 solution is supplemented into the overflow flask, and the micro plastic with the density less than that of the X1 solution is converged into a No. 1 liquid storage bottle (conical bottle) through an overflow pipe 14. This step was repeated three times. Collecting three times to obtain substantially all the micro-plastics (density is less than 1.0 g/cm) with density less than that of the X1 solution in the water sample3Micro plastic of (e), i.e., polyethylene).
5. Next, the first valve 5 is closed and the second valve 7 and the third valve 12 are opened. Starting the high-pressure air pump 15, injecting high-pressure air into the return pipeline, and spraying the residual liquid in the separation pipeline to the separation starting point (in the pipeline between the sample inlet 1 of the separation pipeline and the first rotary nozzle 3) along the return pipeline. The rest of the micro-plastics with other density in the liquid is collected by the reversible screen 4, and the filtered X1 solution is totally sent into the waste liquid cylinder 17 through the waste liquid pipe 11, and the first step of collection is completed.
6. And (3) carrying out second-step collection: and (3) replacing the X1 solution in the high-pressure fluid infusion flusher 9 with an X2 solution, repeating the steps 2-5, collecting the micro plastic (polystyrene) with the density being more than that of the X1 solution and less than that of the X2 solution, and filling the micro plastic (polystyrene) into a No. 2 liquid storage bottle.
7. And (5) carrying out third-step collection: the X2 solution in the high-pressure fluid infusion flusher 9 is changed into X3 solution, so that the micro plastic (polyester) with the density larger than that of the X2 solution and smaller than that of the X3 solution can be collected and put into a No. 3 liquid storage bottle.
8. And (5) carrying out the fourth step of collection: the X3 solution in the high-pressure fluid infusion flusher 9 is changed into X4 solution, so that the micro plastic (artificial fiber) with the density larger than that of the X3 solution and smaller than that of the X4 solution can be collected and put into a No. 4 liquid storage bottle.
9. After the collection of the micro-plastics with various densities is finished, starting a water bath constant temperature oscillator 19, adjusting the water temperature to 45 ℃, putting the micro-plastics into a No. 1-4 liquid storage bottle, setting the oscillation speed to be 80rpm and the oscillation time to be 24h, after full oscillation, respectively carrying out suction filtration on the micro-plastics in the liquid storage bottles to 0.7 mu m filter membranes (GF/F,
Figure BDA0003241893660000101
whatman), the filters were placed in glass petri dishes and air dried at room temperature to be tested.
Observation and counting of the micro-plastics:
the membrane-bound microplastics were visualized with a stereomicroscope (M165C, Leica, Germany) at a magnification of 160, and suspected microplastics were determined based on previously established microplastic Identification standards (Hidalgo-Ruz V, Gutow L, Thompson R C, et al. microplasms in the Marine Environment: A Review of the Methods Used for Identification and Quantification [ J ]. Environmental Science and Technology, 30646 (6): 0-.
In order to ensure that the micro plastic is not polluted by the outside world in the collection, treatment and analysis processes, the sampling container and the experimental instrument are cleaned for three times by ultrapure water before each experiment, the experiment table and the body type microscope are wiped by alcohol, and the surface of the micro plastic is covered by aluminum foil after each step is completed in the experiment process. The operator wears the cotton test clothes in the whole process of the experiment.
The experimental results are shown in table 1, the collection numbers of polyethylene, polystyrene, polyester and rayon are 20, 19 and 18 respectively, and the total collection rate is between 90% and 100%. Therefore, the continuous separation device for the micro-plastics with different densities has higher collection rate, and can efficiently and accurately separate and collect the micro-plastics with different densities in a water sample.
TABLE 1. Collection of the microplastics of the respective densities
Figure BDA0003241893660000102
Figure BDA0003241893660000111
Application example
In order to more intuitively embody the separation effect and the practical value of the continuous separation device, a water body sample is collected in the Wulian sea, and the abundance and the proportion of different-component micro-plastics in the lake water body are researched by utilizing the continuous separation device.
1. Sample collection and analysis
According to the survey specifications of water environment and lake wetland in China, the distribution and hydrodynamic characteristics of the discharge of the Wuliang vegetarian sea into the lake outlet are considered at the same time, the Wuliang vegetarian sea is subjected to square gridding in space by taking 2km multiplied by 2km as a scale, and 5 sample collection points (I12, L15, N13, O10 and S6 are arranged at the intersection points of the square grids from north to south). The sample collection time is 2020 and 9 months, a vacuum pump is adopted to pump 50cm of water below the water surface into a high-density polyethylene bottle with the volume of 1 liter, and three times of sampling points are set.
According to previous research, the micro-plastics in the Wuliang plain sea are mainly polybutylene terephthalate, polystyrene and polyethylene, and the density is 1.40g/cm3，1.05g/cm3And 0.96g/cm3. Based on the configuration, different density solutions are prepared: the density was 1.0g/cm3Distilled water of (2) having a density of 1.2g/cm3A saturated sodium chloride solution of 1.5g/cm in density3The potassium formate solution of (1). Then, the continuous separation device of the invention is used for separating, identifying and counting the micro-plastics with different densities according to the separation process in the experimental example.
It should be noted that the quantity of the micro-plastics with different densities separated from the lake is large, and in order to verify the separation effect of the continuous separation device, 10 samples are randomly selected from the collected micro-plastics with each density for Fourier infrared spectrum detection, and the wave number range is 8000cm-1-50cm-1And comparing the infrared spectrogram with the standard spectrogram of the sample, carrying out qualitative analysis on the target object, and finally determining the quantity of the particles with the components of the micro plastic.
2. Results of the experiment
As shown in FIG. 4, in 5 sample collection points (I12, L15, N13, O10, S6), the abundance of polyethylene varies between 110-. Wherein the percentage of polyethylene in each point varies from 14.19 to 52.41%, the percentage of polystyrene varies from 21.79 to 49.55%, and the percentage of polybutylene terephthalate varies from 17.31 to 48.71%. The ratio of the various micro-plastics is relatively close in variation range, which indicates that the abundance of the three micro-plastics in the Wulian sea is not very different.
Fourier transform infrared spectroscopy (FT-IR) has been widely used for identification of micro-plastic components due to its extremely high reliability in analyzing unknown plastic materials. We randomly selected 10 samples from each of the three densities of the micro-plastics for fourier transform infrared spectroscopy. The results showed that the 10 selected densities were less than 1.0g/cm3The micro-plastic has 9 polyethylene, and 10 selected density ranges from 1.0-1.2g/cm3The micro-plastics are all polystyrene, and 10 selected density ranges are 1.2-1.5g/cm 38 of the micro-plastics are polybutylene terephthalate. Typical FT-IR spectra of these three plastic polymers are shown in FIGS. 5-7. In general, the detection result shows that the device of the invention has good collection effect on micro-plastics of different types (densities). There are individual micro-plastics that are not micro-plastics of the corresponding density, probably because small amounts of other types of plastic substances are identified as micro-plastics in the batch identification, which is quite common in the identification of micro-plastics.
The above embodiments are only some, not all embodiments of the present invention. The above examples are only for explaining and illustrating the technical solutions of the present invention, and are not intended to limit the scope of the present invention. Any modification or variation of the above-described embodiments within the technical scope of the present disclosure by those skilled in the art should be covered by the protection scope of the present disclosure.

Claims (10)

1. The continuous separation device for the micro-plastics with different densities is characterized by comprising a separation pipeline and a return pipeline which are communicated with each other in a gas-liquid mode;
the upper end of the separation pipeline is provided with a sample inlet (1), and the lower end of the separation pipeline is provided with a high-pressure gas inlet (2); a first rotary spray nozzle (3), a reversible screen (4), a first valve (5), a second rotary spray nozzle (6), a second valve (7) and a third rotary spray nozzle (8) are sequentially arranged in a pipeline between the sample inlet (1) and the high-pressure gas inlet (2) from top to bottom;
wherein the first rotating nozzle (3), the second rotating nozzle (6) and the third rotating nozzle (8) are externally connected with a high-pressure fluid infusion flusher (9); a waste liquid outlet (10) is arranged on a pipeline between the reversible screen (4) and the first valve (5), the waste liquid outlet (10) is externally connected with a waste liquid pipe (11), and a third valve (12) is arranged in the waste liquid pipe (11); an overflow port (13) is arranged on a pipeline between the second rotary spray head (6) and the second valve (7), and the overflow port (13) is externally connected with an overflow pipe (14);
an opening at the upper end of the return pipeline is arranged on a pipeline between the sample inlet (1) and the first rotary spray head (3); the lower end of the return pipeline is communicated with the lower end of the separation pipeline; the high-pressure air inlet (2) faces the return pipeline and is externally connected with a high-pressure air pump (15).
2. Continuous separation device according to claim 1, characterized in that the conduit between the second rotary sprayer (6) and the overflow (13) is interrupted, where a conical funnel (16) is provided; the opening at the upper end of the funnel body of the conical funnel (16) is right opposite to the pipe orifice below the second rotary spray head (6), and the lower end of the neck of the conical funnel (16) extends into the pipe orifice above the overflow port (13).
3. Continuous separation device according to claim 1, characterized in that the conduit between the overflow (13) and the second valve (7) and close to the second valve (7) is expanded spherically.
4. Continuous separation device according to claim 1, characterized by further comprising a waste liquid cylinder (17) and a liquid storage bottle (18); the water outlet of the waste liquid pipe (11) is communicated with a waste liquid cylinder (17); the water outlet of the overflow pipe (14) leads to a liquid storage bottle (18).
5. Continuous separation device according to claim 1, characterized in that it further comprises a water bath thermostatic oscillator (19) and a vacuum filtration device (20).
6. Continuous separation apparatus according to any one of claims 1 to 5, characterised in that the pipes of the separation line and the return line are made of stable glass.
7. Method for the separation of microplastics of different densities from a sample, characterized in that a continuous separation device according to any of claims 1-6 is used for the separation of microplastics of different densities from a sample of water.
8. The method of claim 7, comprising the steps of:
s1, closing a first valve (5) and a second valve (7), and opening a third valve (12); adding a water sample to be detected into the sample inlet (1), enabling the liquid to flow downwards and be filtered by the reversible screen (4), intercepting micro plastic in the liquid by the reversible screen (4), and discharging the filtrate through the waste liquid pipe (11);
s2, closing the second valve (7) and the third valve (12), and opening the first valve (5); turning over the reversible screen (4) to enable the surface of the micro-plastic-loaded screen to face downwards;
s3, adding a first solution into the high-pressure fluid infusion flusher (9), enabling an opening of the first rotary spray head (3) to face downwards and an opening of the second rotary spray head (6) to face upwards, then alternately using the first rotary spray head (3) and the second rotary spray head (6) to flush the reversible screen (4), and completely flushing the entrapped micro-plastic;
s4, standing to enable the micro plastic with the density larger than that of the first solution to be precipitated; opening a second rotary spray head (6), supplementing a first solution into the pipeline, and enabling the micro plastic with the density smaller than that of the first solution to flow into a liquid storage bottle (18) through an overflow port (13);
s5, closing the first valve (5), and opening the second valve (7) and the third valve (12); starting a high-pressure air pump (15), pressing residual liquid in the separation pipeline into a return pipeline through high-pressure air, and making the residual liquid return to the upper end of the separation pipeline; the residual liquid is filtered by the reversible screen (4), the residual micro-plastic is retained by the reversible screen (4), and the filtrate is discharged through the waste liquid pipe (11);
s6, replacing the first solution in the high-pressure fluid infusion flusher (9) with a second solution with higher density, and repeating the steps S2-S5 to collect the micro plastic with the density higher than that of the first solution and lower than that of the second solution; and the operation is carried out until micro plastics in various density ranges in the water sample are collected.
9. The method of claim 8, further comprising the step of:
and S7, starting a water bath constant temperature oscillator (19), fully oscillating the micro plastic suspension in each liquid storage bottle (18), respectively filtering the micro plastic in each density range to a filter membrane by using a vacuum filtering device (20) after oscillation is finished, putting the filter membrane into a glass culture dish, and air-drying at room temperature to be detected.
10. Method for determining the abundance of a micro-plastic in a sample, characterized in that micro-plastics of different densities in a sample are separated using the method according to any of claims 7 to 9, and then the micro-plastics of different densities are subjected to component identification and enumeration.
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CN111231172A (en) * 2020-01-17 2020-06-05 河海大学 High-precision separation and recovery system for micro-plastics in open water sediments and application thereof

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Publication number Priority date Publication date Assignee Title
CN109049426A (en) * 2018-08-30 2018-12-21 泸州市龙马潭区鑫泉泡沫塑料有限责任公司 A kind of foamed plastics crushing reclaimer
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