CN108837951A - Micro- plastics separating flotation device and method in a kind of ambient soil and sediment sample - Google Patents

Micro- plastics separating flotation device and method in a kind of ambient soil and sediment sample Download PDF

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Publication number
CN108837951A
CN108837951A CN201810604532.4A CN201810604532A CN108837951A CN 108837951 A CN108837951 A CN 108837951A CN 201810604532 A CN201810604532 A CN 201810604532A CN 108837951 A CN108837951 A CN 108837951A
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micro
flotation
plastics
sediment sample
separating flotation
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卢学强
韩晓昕
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Nankai University
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Nankai University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00Flotation
    • B03D1/14Flotation machines
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q

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  • Engineering & Computer Science (AREA)
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  • Health & Medical Sciences (AREA)
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Abstract

The invention belongs to the pre-treatment research fields of environmental contaminants, are related to the separating flotation device and method of micro- plastics, especially for the separating flotation of micro- plastic grain in ambient soil and sediment sample.The inventive system comprises separate reactor and filter two parts, carry out separating flotation to micro- plastic grain in soil or sediment sample using aeration and the method for overflow.The device of the invention is simple, easy to operate, time-consuming short and efficient, solves cumbersome, the deficiency that time-consuming in the micro- plastics separating flotation method of tradition.In addition, flotation fluid high-efficiency and economic selected by the present invention and can be recycled, save the cost while, reduces environmental pollution.

Description

Micro- plastics separating flotation device and method in a kind of ambient soil and sediment sample
Technical field
The invention belongs to the pre-treatment research fields of environmental contaminants, are related to the separating flotation device and method of micro- plastics, Especially for the separating flotation of micro- plastic grain in ambient soil and sediment sample.
Background technique
Micro- one word of plastics was put forward for the first time in 2004 by the Thompson of Britain, was for describing less than 50 microns at that time Plastic grain(Thompson, R. C. etc., Lost at Sea: Where is All the Plastic Science, 2004, 304, 838.).2009, in relation to plastics ocean rubbish appearance, influence and return the international Conference to become On, Arthur proposes that " micro- plastics " should include all particles less than 5 millimeters.Do not have also to the size of " micro- plastics " so far There is specific definition, most people generally accepts it for plastic grain of the partial size less than 5 millimeters, but intuitively, and partial size is small In the definition of 1 millimeter more compound " micro- plastics ", and Browne is sent out by studying the ocean fragment on Tianma Ship river mouth sandy beach Now the plastic grain wherein less than 1 millimeter accounts for 65%(Browne, M.A. etc., Spatial patterns of plastic debris along estuarine shorelines. Environmental Science & Technology, 2010, 3404-3409.).
Plastic product since mid-twentieth century, with the continuous development of synthesis high molecular material, in global range It is being increasing.Since plastics performance is excellent, have the characteristics that light, chemical property is stable, good wearability, at low cost, Therefore it is widely used in life and industrial production rapidly.Due to plastic products it is a large amount of use and waste plastic it is improper Disposition, causes plastic pollution to get worse.Waste plastic exposure in air, by between ultraviolet irradiation, plastics mechanical collision, The effects of biological uptake, will split into smaller plastic grain, thus form micro- plastics.Micro- plastics are due to small volume, easily It is eaten by mistake by different kind organism, it is also possible to which human health is threatened by food chain.Except this, all kinds of toxic additions that contain in micro- plastics It if agent can be discharged into environment, can cause environmental pollution, harm generated to the mankind and other biological.
Up to now in the presence for detecting micro- plastics more than the world in the water body on ground, soil and deposit, or even in north A large amount of micro- plastic grain is detected in the bottom sediment of the 5570 meters of depths in ice ocean(Bergmann, M. etc., High Quantities of Microplastic in Arctic Deep-Sea Sediments from the HAUSGARTEN Observatory. Environmental Science &Technology, 2017, 11000-11010.).2012 with Before, the flotation of micro- plastics mostly uses greatly traditional artificial screening and flotation mode in environmental sample(Hidalgo-Ruz, V. etc., Microplastics in the Marine Environment: A Review of the Methods Used for Identification and Quantification. Environmental Science &Technology, 2012, 3060-3075.), occur some slightly improved micro- flotation of Plastics methods in recent years, such as " the two of the proposition of Germany Nuelle Footwork " extracts micro- plastic grain in sediment sample(Nuelle, M. etc., A New Analytical Approach for Monitoring Microplastics in Marine Sediments.Environmental Pollution, 2013, 161-169.)Deng, but there are the disadvantages of cumbersome, time-consuming for these methods.Therefore, a kind of easy to operate, quick height is studied The device and method that micro- plastics are isolated on effect ground from environmental sample is necessary to micro- plastic pollution correlation exploratory development in future 's.
Summary of the invention
The purpose of the present invention is to propose to separate in a kind of slave ambient soil and sediment sample easy to operate, rapidly and efficiently The device and method of micro- plastics out makes up cumbersome, the deficiency that time-consuming in conventional method.
To achieve the above object, the present invention adopts the following technical scheme that:
Micro- plastics separating flotation device in a kind of ambient soil and sediment sample, it is characterized in that:Including separate reactor part (One)And filter-portion(Two), wherein
Separate reactor part(One)Including:Column reactant 6, air pump 3, gas flowmeter 4, aeration head 7, flowing water Valve 8, Outlet pipe 13, inlet valve 5, water inlet pipe 12, peristaltic pump 2, liquid storing cup 1;It is anti-that flowing water Valve 8 with inlet valve 5 is respectively positioned on column It answers on 6 side wall of body, aeration head 7 is placed in bottom in column reactant 6, and gas flowmeter 4 is between air pump 3 and aeration head 7 On connected pipeline, 2 one end of peristaltic pump is connected by water inlet pipe 12 with inlet valve 5, in other end insertion liquid storing cup 1 liquid level with Under, its object is to the flotation fluid in liquid storing cup is pumped into column reactant.13 one end of outlet pipe is connected to flowing water Valve 8 On, the other end naturally droops;Its object is to by the lesser mass transfer of the density of upper layer flotation fluid and its carrying to filter Part.
Filter-portion(Two)Including:Filter membrane 9, returnable bottle 10, vacuum filtration pump 11;Filter membrane 9 is located at 13 lower end of outlet pipe, Returnable bottle 10 is connected with vacuum filtration pump 11 by pipeline.
Micro- plastics separating flotation device in ambient soil and sediment sample of the present invention, the column reactant 6 Inside is equipped with flow structure 14, and its object is to so that the lesser micro- plastics of density and other substances in the flotation fluid of upper layer is passed through the knot Structure is more convenient for collecting.
The pipeline being connected between air pump 3 of the present invention and aeration head 7, one end are connect with the air pump 3, the other end with Aeration head 7 connects.The pipeline being connected between returnable bottle 10 and vacuum filtration pump 11, one end connect with the air exhaust nozzle on returnable bottle 10 It connects, the other end is connect with vacuum filtration pump 11.
The present invention further discloses plastics separating flotation device micro- in the ambient soil and sediment sample progress Separating flotation method, it is characterised in that:Using aeration and the method for overflow to micro- plastic grain in soil or sediment sample Carry out separating flotation.Firstly, flowing water Valve is in close state, required flotation fluid is poured into column reactant, by air pump It opens, adjusting gas flow meter is passed through constant gas, makes gas be dispersed into minute bubbles by aeration head and be discharged into flotation fluid In;Then, sample is slowly poured into from column reactant top, after sample all pours into, starts peristaltic pump, it will be in liquid storing cup Solution is pumped into a part to column reactant, opens flowing water Valve while starting peristaltic pump, upper layer flotation fluid carries close Low substance is spent by flow structure, is flowed out of the water outlet pipe to the filter membrane of lower section, is vacuumized with vacuum filtration pump, then use Cleaning solution washes away alkali, finally, the residue on filter membrane is collected, using in residue on naked eyes or Stereo microscope observation filter membrane Micro- plastic grain.Filtrate after vacuumizing is collected in returnable bottle, is reused.The cleaning solution is deionized water.It is described Flotation fluid be saturated sodium chloride solution, density be 1.2 g/cm3, saturation IodineSodium Solution, density be 1.8 g/cm3By volume Than 1:1 mixed solution;The cleaning solution is deionized water;The aperture of the filter membrane is 0.45 micron.
The present invention further disclose in the ambient soil and sediment sample micro- plastics separating flotation device into Application of the row separating flotation method in terms of rapidly isolating micro- plastic grain from soil or sediment sample.Experimental result Display apparatus of the present invention and method can complete first separation flotation in 10 minutes, and separating flotation effect is fine.
Present invention mainly solves plastics separating flotation method micro- in existing soil and sediment sample is cumbersome, time-consuming The problems such as long, main difficult point are that i.e. time saving and efficiently separating flotation comes out from sample by micro- plastic grain, thus first Investigated aeration condition afterwards, the conditions such as saturated sodium chloride solution and the volume ratio for being saturated IodineSodium Solution in flotation fluid, it is last really Determine above-mentioned apparatus and method.
Micro- plastics separating flotation device and method and the prior art in ambient soil and sediment sample disclosed by the invention It is compared to possessed good effect:
(1)The invention proposes a kind of methods of aeration and overflow to divide micro- plastic grain in soil or sediment sample From flotation, and devise related separating flotation device.The device is easy to operate, can be efficiently and rapidly from soil or deposit Micro- plastic grain is isolated in sample, solves the deficiencies of micro- plastics separating flotation method of tradition is cumbersome, time-consuming, this hair Bright device separate reactor part and filter two parts composition.Only flotation fluid need to be added, be passed through gas, pour into sample again Rapidly isolate micro- plastic grain in sample.
(2)It is applied widely.The device of the invention and method are to the separating flotation from ambient soil and sediment sample Micro- plastic grain is applicable in, and is suitable for separating a plurality of types of micro- plastics.
(3)It is economical, at low cost.The flotation fluid and other solution of device low manufacture cost, selection designed by the present invention at This is cheap, relatively inexpensive.
(4)It is environmentally friendly.The material of device designed by the present invention and the flotation fluid of selection and other solution are nontoxic Harmless, environmental pollution is smaller, and flotation fluid is reusable, reduces pollution of the solution to ambient enviroment.
Detailed description of the invention
Fig. 1 is micro- plastics separating flotation device figure in ambient soil provided by the invention and sediment sample;
Wherein:1 liquid storing cup;2 peristaltic pumps;3 air pumps;4 gas flowmeters;5 inlet valves;6 column reactants;7 aeration heads;8 Flowing water Valve;9 filter membranes;10 returnable bottles;11 vacuum filtration pumps;12 water inlet pipes;13 outlet pipes;14 flow structures.
Specific embodiment
The present invention is described below by specific embodiment.Unless stated otherwise, technological means used in the present invention It is method known in those skilled in the art.In addition, embodiment is interpreted as illustrative, it is not intended to limit the present invention Range, the spirit and scope of the invention are limited only by the claims that follow.To those skilled in the art, without departing substantially from this Under the premise of invention spirit and scope, to the various changes or change of material component and dosage progress in these embodiments It belongs to the scope of protection of the present invention.The raw materials used in the present invention and reagent are commercially available.
Embodiment 1
Micro- plastics separating flotation device in a kind of ambient soil and sediment sample, including separate reactor part(One)And filtering Device part(Two), wherein
Separate reactor part(One)Including:Column reactant 6, air pump 3, gas flowmeter 4, aeration head 7, flowing water Valve 8, Outlet pipe 13, inlet valve 5, water inlet pipe 12, peristaltic pump 2, liquid storing cup 1;It is anti-that flowing water Valve 8 with inlet valve 5 is respectively positioned on column It answers on 6 side wall of body, aeration head 7 is placed in bottom in column reactant 6, and gas flowmeter 4 is between air pump 3 and aeration head 7 On connected pipeline, 2 one end of peristaltic pump passes through water inlet pipe 12 and inlet valve(5)Be connected, the other end be inserted into liquid storing cup liquid level with Under, the flotation fluid in liquid storing cup is pumped into column reactant, 13 one end of outlet pipe is connected on flowing water Valve 8, and the other end is certainly So sagging, the purpose is to by the lesser mass transfer of the density of upper layer flotation fluid and its carrying to filter-portion;
Filter-portion(Two)Including:Filter membrane 9, returnable bottle 10, vacuum filtration pump 11;Filter membrane 9 is located at 13 lower end of outlet pipe, recycling Bottle is connected with vacuum filtration pump by pipeline.Flow structure 14 is equipped with inside column reactant, effect is to make upper layer flotation fluid The middle lesser micro- plastics of density and other substances with this configuration, are more convenient for collecting.It is connected between air pump 3 and aeration head 7 Pipeline, one end are connect with the air pump, and the other end is connect with aeration head.
Embodiment 2
The present invention carries out separating flotation simultaneously to micro- plastic grain in soil or sediment sample using aeration and the method for overflow Design corresponding separating flotation device.Concrete operations are as follows:
Micro- plastics separating flotation device in a kind of ambient soil and sediment sample, including separate reactor part and filter Part, wherein separate reactor part includes column reactant, air pump, gas flowmeter, aeration head, flowing water Valve, water outlet Pipe, inlet valve, water inlet pipe, peristaltic pump, liquid storing cup, filter-portion include filter membrane, returnable bottle and vacuum filtration pump.It is described go out Penstock is respectively positioned on column with inlet valve and reacts on body sidewall;The aeration head is put in bottom in column reactant;The gas On the pipeline that flowmeter body is connected between air pump and aeration head;The filter membrane is located at outlet pipe lower end;The returnable bottle It is connected with vacuum filtration pump by pipeline.Flow structure is equipped with inside the column reactant.
The peristaltic pump, one end are connected by water inlet pipe with inlet valve, and the other end is inserted into liquid storing cup below liquid level.
The pipeline being connected between the air pump and aeration head, one end are connect with the air pump, and the other end and aeration head connect It connects.
The pipeline being connected between the returnable bottle and vacuum filtration pump, one end is connect with the air exhaust nozzle on returnable bottle, another End and vacuum filtration pump connection.The outlet pipe, one end are connected on flowing water Valve, and the other end naturally droops.
Embodiment 3
A kind of micro- plastics separating flotation method in ambient soil and sediment sample, using aeration and the method for overflow to soil or Micro- plastic grain in sediment sample carries out separating flotation.Firstly, flowing water Valve is in close state, required flotation fluid is fallen Enter in column reactant, air pump is opened, adjusting gas flow meter is passed through constant gas, makes gas by aeration head Minute bubbles are dispersed into be discharged into flotation fluid;Then, sample is slowly poured into from column reactant top, sample all pours into Afterwards, continue to be aerated certain time, start peristaltic pump, the solution in liquid storing cup is pumped into a part to column reactant, starting Flowing water Valve is opened while peristaltic pump, upper layer flotation fluid carries low density substance by flow structure, from outlet pipe stream It out on the filter membrane of lower section, is vacuumized with vacuum filtration pump, then wash away alkali with cleaning solution, finally, collecting on filter membrane Residue utilizes micro- plastic grain in residue on naked eyes or Stereo microscope observation filter membrane.
Wherein the aperture of filter membrane is 0.45 micron.Flotation fluid is saturated sodium chloride solution(Density is 1.2 g/cm3)With it is full And IodineSodium Solution(Density is 1.8 g/cm3)By volume 1:0 mixed solution, as pure saturated sodium chloride solution;Clearly Washing lotion is deionized water.Filtrate after vacuumizing is collected in returnable bottle, is reused.
Wherein the uninterrupted of gas is carried out by the gas flowmeter being connected between air pump and air inlet pipe on pipeline It adjusts and measures.It is passed through constant air-flow by air pump and gas flowmeter, minute bubbles are converted for gas by aeration head It is uniformly discharged into column to react in intracorporal flotation fluid, the micro- plastic grain and color density in sample are lower than flotation fluid density Substance with upper liquid together from flowing water Valve flow out, by outlet pipe flow to lower section filter membrane on, vacuum makes Flotation fluid enters in the returnable bottle of lower section, reuses after collection.
Embodiment 4
The concrete operation step of separating flotation process is as follows:
Step 1:The pedotheque of field acquisition is dried(Lower than 60 DEG C)Processing, is filtered with the sieve in the aperture 1mm, Then the micro- plastic grain of whole therein is removed, the polypropylene after taking 200g treated pedotheque incorporation grinding(PP)Micro- modeling Expect particle(About 0.22657 g of quality, diameter are respectively less than 1mm), it is uniformly mixed.
Step:2:The saturated sodium chloride solution for preparing 1.3L, is all poured into column reactant.
Step 3:It opens air pump and is passed through constant air-flow into column reactant, adjust air flow meter and make gas stream Speed is 2 L/min, by aeration head gas is dispersed into after minute bubbles are discharged into flotation fluid, by step 1 treated sample Product are slowly all poured into from column reactant top.
Step 4:Continue to be aerated 30 s, close air pump, starts peristaltic pump(Flow velocity:0.09 L/min), will be in liquid storing cup Flotation fluid(Saturated sodium chloride solution)It is pumped into column reactant.
Step 5:While starting peristaltic pump, open flowing water Valve, the lower substance of density with upper layer flotation fluid By flow structure, it is flow to from flowing water Valve by outlet pipe on the filter membrane of lower section.
Step 6:While flotation fluid flow to filter membrane on upper layer, vacuum filtration pump is opened, after upper layer flotation fluid all flows out, Deionized water is directly poured on filter membrane, is continued to filter, is washed away alkali.
After flotation substance on filter membrane is further processed, micro- plastic grain therein is sorted out, weighing its quality is 0.22239g, the rate of recovery for calculating micro- plastics separating flotation method is 98%.
Embodiment 5
Micro- plastics kind after incorporation processing in pedotheque is polyethylene terephthalate(PET), flotation fluid is saturation chlorine Change sodium solution(Density is 1.2 g/cm3)With saturation IodineSodium Solution(Density is 1.8 g/cm3)By volume 1:1 mixing it is molten Liquid, other steps are same as Example 3, and calculating its rate of recovery is 96%.
Therefore, when carrying out carrying out separating flotation to plastics micro- in actual sample, flotation fluid uses saturated sodium chloride solution (Density is 1.2 g/cm3)With saturation IodineSodium Solution(Density is 1.8 g/cm3)By volume 1:1 mixed solution.With it is current Micro- plastics separating flotation device and method is compared in other existing soil or sediment sample, such as one kind of landblink China proposition Micro- flotation of Plastics separator and its application, only stirring and be aerated in step needs 15 minutes, and micro- plastics of the propositions such as Zhang Kai Separation method and device need to stir at least 30 minutes, be carried out using the device of the invention and method to soil and sediment sample micro- Plastics separating flotation whole operation process only needs 10 minutes, and the high efficiency of method is in turn ensured while shortening the time(Add Marking the rate of recovery is 96% -98%).
In addition, the flotation fluid of existing micro- plastics separating flotation method is mostly pure saturated sodium chloride solution or full at present And IodineSodium Solution, or utilize two-step method, first use saturated sodium chloride solution, then be saturated IodineSodium Solution.The method of the present invention Using the mixed solution of the two, efficiently micro- plastics in sample not only can be gone out by separating flotation, but also solve simple saturation chlorine Change sodium solution can not floatingly select the biggish micro- plastic grain of density and simple saturation IodineSodium Solution economic cost is too high Problem, and do not need to increase cumbersome operation using two-step method.
To sum up, micro- plastics separating flotation device and method can in a kind of ambient soil and sediment sample proposed by the present invention I.e. rapidly and efficiently by micro- plastic grain, separating flotation is come out from sample, and save cost, it is relatively inexpensive, have stronger Scientific research and commercial practicability.

Claims (7)

1. micro- plastics separating flotation device in a kind of ambient soil and sediment sample, it is characterized in that:Including separate reactor portion Point(One)And filter-portion(Two), wherein
Separate reactor part(One)Including:Column reactant(6), air pump(3), gas flowmeter(4), aeration head(7), go out Penstock(8), outlet pipe(13), inlet valve(5), water inlet pipe(12), peristaltic pump(2), liquid storing cup(1);Flowing water Valve(8)With Inlet valve(5)It is respectively positioned on column reactant(6)On side wall, aeration head(7)It is placed in column reactant(6)Interior bottom, gas stream Meter(4)Positioned at air pump(3)With aeration head(7)Between be connected pipeline on, peristaltic pump(2)One end passes through water inlet pipe(12)With Inlet valve(5)It is connected, the other end is inserted into liquid storing cup(1)Liquid level is hereinafter, be pumped into column reactant for the flotation fluid in liquid storing cup (6)In, outlet pipe(13)One end is connected to flowing water Valve(8)On, the other end naturally droops, by upper layer flotation fluid and its carrying The lesser mass transfer of density is to filter-portion;
Filter-portion(Two)Including:Filter membrane(9), returnable bottle(10), vacuum filtration pump(11);Filter membrane(9)Positioned at outlet pipe (13)Lower end, returnable bottle(10)It is pumped with vacuum filtration(11)It is connected by pipeline.
2. micro- plastics separating flotation device, feature in a kind of ambient soil according to claim 1 and sediment sample It is:The column reactant(6)Inside is equipped with flow structure(14), make in the flotation fluid of upper layer the lesser micro- plastics of density and its His substance with this configuration, is more convenient for collecting.
3. micro- plastics separating flotation device, feature in a kind of ambient soil according to claim 1 and sediment sample It is:The air pump(3)With aeration head(7)Between the pipeline that is connected to, one end and the air pump(3)Connection, the other end and exposure Gas head(7)Connection.
4. micro- plastics separating flotation device, feature in a kind of ambient soil according to claim 1 and sediment sample It is:Returnable bottle(10)It is pumped with vacuum filtration(11)Between the pipeline that is connected to, one end and returnable bottle(10)On air exhaust nozzle connection, The other end and vacuum filtration pump(11)Connection.
5. a kind of separated using micro- plastics separating flotation device in ambient soil described in claim 1 and sediment sample Method for floating, it is characterised in that:Firstly, flowing water Valve is in close state, required flotation fluid is poured into column reactant, it will Air pump is opened, and adjusting gas flow meter is passed through constant gas, makes gas be dispersed into minute bubbles by aeration head and be discharged into In flotation fluid;Then, sample is slowly poured into from column reactant top, after sample all pours into, starts peristaltic pump, by liquid storage Solution in cup is pumped into a part to column reactant, opens flowing water Valve while starting peristaltic pump, upper layer flotation fluid is taken It with low density substance by flow structure, flows out of the water outlet pipe to the filter membrane of lower section, take out with vacuum filtration pump true Sky, then alkali is washed away with cleaning solution, finally, the residue on filter membrane is collected, using on naked eyes or Stereo microscope observation filter membrane Micro- plastic grain in residue;The flotation fluid is saturated sodium chloride solution and saturation IodineSodium Solution by volume 1:1 Mixed solution;The cleaning solution is deionized water;The aperture of the filter membrane is 0.45 micron.
6. separating flotation method described in claim 5, it is characterised in that the filtrate after vacuumizing is collected in returnable bottle, and repetition makes With.
7. carrying out separating flotation using micro- plastics separating flotation device in ambient soil and sediment sample described in claim 5 Application of the method in terms of rapidly isolating micro- plastic grain from soil or sediment sample.
CN201810604532.4A 2018-06-13 2018-06-13 Micro- plastics separating flotation device and method in a kind of ambient soil and sediment sample Pending CN108837951A (en)

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