CN108254284A - A kind of method of micro- plastic content in detection water body - Google Patents
A kind of method of micro- plastic content in detection water body Download PDFInfo
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- CN108254284A CN108254284A CN201810273758.0A CN201810273758A CN108254284A CN 108254284 A CN108254284 A CN 108254284A CN 201810273758 A CN201810273758 A CN 201810273758A CN 108254284 A CN108254284 A CN 108254284A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
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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
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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
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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
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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
- G01N1/40—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
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Abstract
The invention discloses a kind of methods for detecting micro- plastic content in water body, and including following methods step, a is carried out carrying out water body using direct selecting method, large sample method or concentration example-based approach first the sampling of science, is then charged into the solvent bottle of 500ml；B removes impurity manually to the water body of sampling；C, processes silver filtering foil and then song is made cylindric, selects the bar that stirs of glass material, then by way of activated carbon powder material magnetron sputtering, will filtering foil it is completely seamless with stirring bar adherency；D, configuration precipitation catalysis reaction solution, then configuration purified solution is poured into the solvent bottle that need to be detected, adequately reacted respectively；E by step d, is filtered by using nanofiltration net, is then collected micro- plastics.The method of the present invention, which is based on saturation stablizing solution, can make micro- plastics float, and make that micro- plastics lock out operation from water body example is simple, and testing cost is low, and new thinking is provided for micro- plastics environment pollution detection.
Description
Technical field
The present invention relates to technical field of environmental purification, especially a kind of method for detecting micro- plastic content in water body.
Background technology
Micro- plastics are commonly defined as：Size is between the plastic granule of 0.2-5.0mm, microfibre, plastic grain, foamed plastics
Or film etc., micro- plastics mainly include equipment breakage and the raw material of sewage discharge, dumping, operation on the sea and Shipping
The processes such as leakage, coastal region mankind's activity bring the plastic particles raw materials of natural environment into, bulk plastic rubbish is made through physics
With the particulate additive in the daily necessities such as the plastic scrap of formation, facial cleanser and polishing material of industrial application etc., into environment
Micro- plastics since grain size is small, density is low, can be migrated under the external force such as wind-force, river, ocean current, micro- plastic nature is opposite
Stablize, can long-term existence in environment, but its surface physicochemical property can change under the effects that sunlight, wind-force, wave；It is micro-
Plastics size is smaller, large specific surface area, hydrophobicity are strong, is the ideal carrier of numerous hydrophobic organic pollutants and heavy metal, micro-
Plastics are easily eaten by mistake by planktonic organism and fish etc., can be detained in organism for a long time, and transfer and enrichment occur in food web,
It constitutes a threat to ecological environment security.
At present, the method for sampling of existing micro- plastics is also there is the place of some shortcomings, such as；Existing micro- plastics
The method of sampling is due to method of sampling difference, and many result of study concentration units represent completely different, it is difficult to which lateral comparison is differently
Micro- plastic pollution degree in area；In addition, different analysis methods in the rate of recovery also difference of sample pretreatment process, lead to phase
The result error for analyzing acquisition in different ways with sample is larger.Micro- plastic pollution problem belongs to global pollution problem, it
Have a very wide distribution in water body, the concentration order of magnitude it is smaller, at present detection method more fall behind, for more than, it is proposed here one
The method of micro- plastic content in kind detection water body.
Invention content
The present invention is solves above-mentioned phenomenon, using the technical solution of following modification, micro- plastic content in a kind of detection water body
Method, including following methods step,
A carries out carrying out water body using direct selecting method, large sample method or concentration example-based approach first the sampling of science, so
It is fitted into the solvent bottle of 500ml afterwards；
B, to the water body of sampling carry out using binocular microscope reject impurity, it will be observed that fiber for threadiness, do not send out
Raw bending, winding, then may be biological source fiber, should give rejecting, and granule boundary must be clear, whole uniform color, if
Grain is white or transparent, needs to utilize the amplification factor of bigger or selection fluorescent marker microscope；
C, processes silver filtering foil and then song is made cylindric, selects the bar that stirs of glass material, then by using activated carbon
The mode of powder material magnetron sputtering, filtering foil is completely seamless with stirring bar adherency；
D, configuration precipitation catalysis reaction solution, then pours into configuration purified solution in the solvent bottle that need to be detected, respectively
The ratio entered is 0.34 by volume：1, then the bar that stirs machined in step c with motor is attached, passes through motor band
It is dynamic to stir bar rotation absorption pond impurity, reaction solution is catalyzed by precipitation and realizes solvent saturation, fully oscillation, stirring is allowed to mix
Uniformly, it then staticly settles until heavy constituent is detached from aqueous phase system and settles again, and micro- plastics continue to keep suspended state or drift
Float on solution surface；
E by step d, is filtered by using nanofiltration net, then filter screen is rinsed with clear water to
In heating bottle, heating bottle is heated, until moisture content is dried, is then collected micro- plastics, and weighed by component, then
The content of micro- plastics is calculated by simple division.
As present invention further optimization mode, the precipitation catalysis reaction solution is concentration expressed in percentage by weight in 85-
The solution of 94% HCl passes through with mixed solution according to 1:1.75 ratio be prepared by fully mixing, the mixed solution packet
Include NAOH, Na2CO3、ZnCO3、NaHCO3、Zn(HCO3)2、Zn(OH)2。
As present invention further optimization mode, the specific deal of the mixed solution is included hereinafter, including 5-10 parts
NAOH, 8-15 part Na2CO3, 6-12 parts of ZnCO3, 5-10 parts of NaHCO3, 3-5 parts of Zn (HCO3) 4-8 parts of Zn
(OH)2。
As present invention further optimization mode, the specific deal of the mixed solution include hereinafter, 10 parts
NAOH, 15 parts of Na2CO3, 12 parts of ZnCO3, 10 parts of NaHCO3, 5 parts of Zn (HCO3), 8 parts of Zn (OH)2。
As present invention further optimization mode, the direct selecting method is straight from environmental sample by naked eyes identification
The method for connecing the micro- plastics of picking, especially grain size are easier to recognize in the sample, direct selecting method is fitted in the plastic granule of 1-6mm
For the acquisition of plastic granule in deposit particularly surface sediment samples, when micro- plastics do not have specific modality structure and with
When other impurities mix, direct selecting method is just difficult to the micro- plastics of picking.
As present invention further optimization mode, the concentration example-based approach refers in sampling location immediately to a large amount of samples
It the extraction operations such as is filtered, sieves, retaining target components so as to the method further analyzed, the screening of sediment sample operates
It can be done directly in sampling location, and the filter operation of seawater sample usually carries out on scientific investigation ship.
As present invention further optimization mode, the large sample method is to be deposited composition granule covering, ring in micro- plastics
Micro- plastics abundance is low in the sample of border, and need to pass through the preprocess methods such as concentration, enrichment can just be detected, and grain size is too small, can not be by meat
Eye observation etc., the acquisition of plastic granule in object particularly surface sediment samples.
As present invention further optimization mode, in step d, the rotating speed of motor is controlled, first controls rotating speed control 15-
45r/min pours into catalytic solution, and then control time 15min carries out fully at the uniform velocity stirring, speed of agitator is set as 80-260r/
min。
As present invention further optimization mode, in step e, when carrying out heating, drying to heating bottle, temperature is kept
At 85-110 DEG C, the duration can coordinate fan to carry out acceleration drying effect in 5-12min.
The method of the present invention, which is based on saturation stablizing solution, can make micro- plastics float, and micro- plastics is made to detach behaviour from water body example
To make simply, testing cost is low, and treatment conditions are mild, and the detection for micro- plastics environmental pollution field provides new thinking, and
Present invention offer is a variety of to devise a variety of method of samplings, avoids the result that same sample analyzes acquisition in different ways and occurs partially
The phenomenon that difference is larger, the whole accuracy for improving micro- plastics detection.
Specific embodiment
Below in conjunction in the embodiment of the present invention, the technical solution in the embodiment of the present invention is clearly and completely retouched
It states, it is clear that described embodiment is only part of the embodiment of the present invention, instead of all the embodiments.Based on the present invention
In embodiment, the every other implementation that those of ordinary skill in the art are obtained without making creative work
Example, shall fall within the protection scope of the present invention.
The present invention provides a kind of technical solution：A kind of method of micro- plastic content in detection water body is walked including following methods
Suddenly,
A carries out carrying out water body using direct selecting method, large sample method or concentration example-based approach first the sampling of science, so
It is fitted into the solvent bottle of 500ml afterwards；
B, to the water body of sampling carry out using binocular microscope reject impurity, it will be observed that fiber for threadiness, do not send out
Raw bending, winding, then may be biological source fiber, should give rejecting, and granule boundary must be clear, whole uniform color, if
Grain is white or transparent, needs to utilize the amplification factor of bigger or selection fluorescent marker microscope；
C, processes silver filtering foil and then song is made cylindric, selects the bar that stirs of glass material, then by using activated carbon
The mode of powder material magnetron sputtering, filtering foil is completely seamless with stirring bar adherency；
D, configuration precipitation catalysis reaction solution, then pours into configuration purified solution in the solvent bottle that need to be detected, respectively
The ratio entered is 0.34 by volume：1, then the bar that stirs machined in step c with motor is attached, passes through motor band
It is dynamic to stir bar rotation absorption pond impurity, reaction solution is catalyzed by precipitation and realizes solvent saturation, fully oscillation, stirring is allowed to mix
Uniformly, it then staticly settles until heavy constituent is detached from aqueous phase system and settles again, and micro- plastics continue to keep suspended state or drift
Float on solution surface；
E by step d, is filtered by using nanofiltration net, then filter screen is rinsed with clear water to
In heating bottle, heating bottle is heated, until moisture content is dried, is then collected micro- plastics, and weighed by component, then
The content of micro- plastics is calculated by simple division.
The precipitation catalysis reaction solution is that the solution of HCl of the concentration expressed in percentage by weight in 85-94% passes through with mixed solution
According to 1:1.75 ratio is prepared by fully mixing, and the mixed solution includes NAOH, Na2CO3、ZnCO3、NaHCO3、Zn
(HCO3)2、Zn(OH)2。
The specific deal of the mixed solution is included hereinafter, including the Na of 5-10 parts NAOH, 8-15 part2CO3, 6-12 parts
ZnCO3, 5-10 parts of NaHCO3, 3-5 parts of Zn (HCO3) 4-8 parts of Zn (OH)2。
As present invention further optimization mode, the specific deal of the mixed solution include hereinafter, 10 parts
NAOH, 15 parts of Na2CO3, 12 parts of ZnCO3, 10 parts of NaHCO3, 5 parts of Zn (HCO3), 8 parts of Zn (OH)2。
The direct selecting method is by the method for naked eyes identification micro- plastics of direct picking from environmental sample, especially grain
Diameter is easier to recognize in the sample in the plastic granule of 1-6mm, and direct selecting method is suitable for deposit particularly surface deposit sample
The acquisition of plastic granule in product, when micro- plastics do not have specific modality structure and are mixed with other impurities, direct selecting method is just
It is difficult to the micro- plastics of picking.
The concentration example-based approach such as refers to immediately to be filtered a large amount of samples in sampling location, sieve at extraction operations, the guarantor
Target components are stayed so as to the method further analyzed, the screening operation of sediment sample can be done directly in sampling location, and extra large
The filter operation of water sample usually carries out on scientific investigation ship.
The large sample method is to be deposited composition granule covering in micro- plastics, and micro- plastics abundance is low in environmental sample, need by
The preprocess methods such as concentration, enrichment can be just detected, and grain size is too small, can not be by naked-eye observation etc., object particularly surface deposit
The acquisition of plastic granule in sample.
In step d, the rotating speed of motor is controlled, rotating speed control 15-45r/min is first controlled, pours into catalytic solution, during control
Between 15min, then carry out fully at the uniform velocity stir, speed of agitator is set as 80-260r/min.
In step e, when carrying out heating, drying to heating bottle, 85-110 DEG C is maintained the temperature at, the duration is in 5-
12min, while fan can be coordinated to carry out acceleration drying effect.
Example one is sampled using direct selecting method, acquires the water body of 1000ml
First, to the water body of sampling carry out using binocular microscope reject impurity, it will be observed that fiber for threadiness, not
It bending, winds, then may be biological source fiber, should give rejecting, granule boundary must be clear, whole uniform color, if
Particle is white or transparent, needs to utilize the amplification factor of bigger or selection fluorescent marker microscope；
Then, it processes silver filtering foil and then song is made cylindric, select the bar that stirs of glass material, then by using activity
The mode of carbon powder material magnetron sputtering, filtering foil is completely seamless with stirring bar adherency；
Secondly, then configuration precipitation catalysis reaction solution pours into configuration purified solution in the solvent bottle that need to be detected respectively,
The ratio poured into is 0.34 by volume：1, then the bar that stirs machined in step c with motor is attached, passes through motor
Bar rotation absorption pond impurity is stirred in drive, and being catalyzed reaction solution by precipitation realizes solvent saturation, and fully oscillation, stirring is allowed to mixed
Close uniform, then staticly settle until heavy constituent is detached from aqueous phase system and settles again, and micro- plastics continue to keep suspended state or
Float on solution surface；
Finally, it by step d, is filtered by using nanofiltration net, then filter screen is rushed with clear water
It is washed till in heating bottle, heating bottle is heated, until moisture content is dried, be then collected micro- plastics, and claimed by component
It takes, then the content of micro- plastics is calculated by simple division, be stirred, the impurity in water is adsorbed.
The content of micro- plastics
The content of other pollutants
Significantly can be seen that this kind of method can detect micro- plastics by table, and can obtain its specifically into
Point.
To sum up, method of the invention, which is based on saturation stablizing solution, can make micro- plastics float, and make micro- plastics from water body example
Lock out operation is simple, and testing cost is low, and treatment conditions are mild, and the detection for micro- plastics environmental pollution field provides new think of
Road, and the present invention provide it is a variety of devise a variety of method of samplings, avoid the knot that same sample analyzes acquisition in different ways
There is the phenomenon that deviation is larger, the whole accuracy for improving micro- plastics detection in fruit.
Finally it should be noted that：The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
To modify to the technical solution recorded in foregoing embodiments or carry out equivalent replacement to which part technical characteristic.
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in the present invention's
Within protection domain.
Claims (9)
- A kind of 1. method for detecting micro- plastic content in water body, it is characterised in that：Including following methods step,A is carried out carrying out water body using direct selecting method, large sample method or concentration example-based approach first the sampling of science, then filled In the solvent bottle for entering 500ml；B, to the water body of sampling carry out using binocular microscope reject impurity, it will be observed that fiber for threadiness, do not occur curved Bent, winding, then may be biological source fiber, should give rejecting, granule boundary must be clear, whole uniform color, if particle is It is white or transparent, it needs to utilize the amplification factor of bigger or selection fluorescent marker microscope；C, processes silver filtering foil and then song is made cylindric, selects the bar that stirs of glass material, then by using activated carbon powder material Expect the mode of magnetron sputtering, filtering foil is completely seamless with stirring bar adherency；D, configuration precipitation catalysis reaction solution, then configuration purified solution is poured into the solvent bottle that need to be detected, pour into respectively Ratio is 0.34 by volume：1, then the bar that stirs machined in step c with motor is attached, is stirred by motor drive Bar rotation absorption pond impurity is catalyzed reaction solution realization solvent saturation by precipitation, and fully oscillation, stirring is allowed to mixing It is even, it then staticly settles until heavy constituent is detached from aqueous phase system and settles again, and micro- plastics continue to keep suspended state or floating In solution surface；E by step d, is filtered by using nanofiltration net, and then filter screen is rinsed to heating with clear water In bottle, heating bottle is heated, until moisture content is dried, is then collected micro- plastics, and weighed by component, then pass through Simple division calculates the content of micro- plastics.
- 2. a kind of method for detecting micro- plastic content in water body according to claim 1, which is characterized in that the precipitation is urged It is that solution of the concentration expressed in percentage by weight in the HCl of 85-94% passes through with mixed solution according to 1 to change reaction solution:1.75 ratio into Row is prepared by fully mixing, and the mixed solution includes NAOH, Na2CO3、ZnCO3、NaHCO3、Zn(HCO3)2、Zn(OH)2。
- 3. a kind of method for detecting micro- plastic content in water body according to claim 2, which is characterized in that the mixing is molten The specific deal of liquid is included hereinafter, including the Na of 5-10 parts NAOH, 8-15 part2CO3, 6-12 parts of ZnCO3, 5-10 parts NaHCO3, 3-5 parts of Zn (HCO3) 4-8 parts of Zn (OH)2。
- A kind of 4. method for detecting micro- plastic content in water body according to claim 3, which is characterized in that institute's mixing The specific deal of solution is included hereinafter, 10 parts of NAOH, 15 parts of Na2CO3, 12 parts of ZnCO3, 10 parts of NaHCO3, 5 parts Zn(HCO3), 8 parts of Zn (OH)2。
- 5. a kind of method for detecting micro- plastic content in water body according to claim 1, which is characterized in that described directly to choose It is by the method for naked eyes identification micro- plastics of direct picking from environmental sample to select method, and especially grain size is in the plastic pellet of 1-6mm Material, is easier to recognize in the sample, and direct selecting method plastic granule suitable for deposit particularly surface sediment samples is adopted Collection, when micro- plastics do not have specific modality structure and are mixed with other impurities, direct selecting method is just difficult to the micro- plastics of picking.
- A kind of 6. method for detecting micro- plastic content in water body according to claim 1, which is characterized in that the concentration sample This law such as refers to immediately to be filtered a large amount of samples in sampling location, sieve at the extraction operations, retains target components so as into one The method for walking analysis, the screening operation of sediment sample can be done directly in sampling location, and the filter operation of seawater sample is led to Often carried out on scientific investigation ship.
- A kind of 7. method for detecting micro- plastic content in water body according to claim 1, which is characterized in that the large sample Method is to be deposited composition granule covering in micro- plastics, and micro- plastics abundance is low in environmental sample, need to pass through the pretreatments sides such as concentration, enrichment Method can be just detected, and grain size is too small, can not be by naked-eye observation etc., and plastic granule adopts in object particularly surface sediment samples Collection.
- 8. a kind of method for detecting micro- plastic content in water body according to claim 1, which is characterized in that in step d, control The rotating speed of motor processed first controls rotating speed control 15-45r/min, pours into catalytic solution, then control time 15min is filled Fast stirring is distributed equally, speed of agitator is set as 80-260r/min.
- 9. a kind of method for detecting micro- plastic content in water body according to claim 1, which is characterized in that in step e, When carrying out heating, drying to heating bottle, 85-110 DEG C is maintained the temperature at, the duration can coordinate fan in 5-12min Carry out acceleration drying effect.
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| CN111514868A (en) * | 2020-04-09 | 2020-08-11 | 华东师范大学 | Magnetic nano carbon, preparation method thereof and application thereof in removing micro plastic in water |
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