CN114486476A - Pretreatment method for detecting polyethylene micro-plastic in liquid sample and application thereof - Google Patents
Pretreatment method for detecting polyethylene micro-plastic in liquid sample and application thereof Download PDFInfo
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Abstract
The invention provides a pretreatment method for detecting polyethylene micro-plastic in a liquid sample and application thereof, wherein the treatment method comprises the following steps: after digesting the liquid sample into a clear digestion solution by using a hydrogen peroxide solution, adding sodium bicarbonate to remove excessive hydrogen peroxide in the digestion solution in a heating and ultrasonic mode, adding ethanol into the digestion solution, and dispersing the agglomerated polyethylene micro-plastic in the digestion solution. The invention can eliminate the interference of organic particles in the pretreatment process of the polyethylene micro-plastic, improve the recovery rate and avoid the influence of the corrosion of the sample on the filter membrane on the counting during the filtration.
Description
Technical Field
The invention belongs to the technical field of safety detection, and particularly relates to a pretreatment method for detecting polyethylene micro-plastic in a liquid sample and application thereof.
Background
Polyethylene is a polymer material with wide application, and is commonly used in the production and living fields of plastic product manufacture, food packaging material, film manufacture and the like. The polyethylene is torn and broken due to factors including physics, natural aging and the like in the processes of storage, transportation and use, and then fragments are generated, wherein the particle particles of the fragments with the particle size of less than 5mm belong to the micro plastic. The micro plastic has large specific surface area, is easy to adsorb toxic and harmful substances, and can cause damage to organisms and the environment. At present, the method for quantitatively detecting the micro-plastics is mainly a microscopic counting method, and instruments used in the method comprise a common optical microscope, a microscopic infrared microscope, a microscopic Raman microscope, a scanning electron microscope and the like. The use of the microscopic counting method requires that the liquid sample eventually be enriched with the micro-plastic on the filter. At present, the pretreatment method of the micro-plastic in the liquid sample mainly comprises a density flotation method and a wet digestion method, the liquid sample is filtered after the treatment by the methods, micro-plastic particles are enriched on a filter membrane, the micro-plastic particles are observed and counted by a micro-counting method, the types of the used filter membrane mainly comprise a fiber filter membrane, a macromolecular filter membrane, a metal filter membrane and the like, and the method is also mainly adopted for detecting the polyethylene micro-plastic in the liquid sample.
The density flotation process is the mildest pretreatment method for treating various substrates, including liquid samples. The application number is CN202110312146.X, the name is "a method for quickly extracting and analyzing micro-plastics in soil based on density separation method", and the micro-plastics are further treated after being floated by using magnesium chloride saturated solution, and finally, the micro-plastics are qualitatively detected. The density flotation method cannot eliminate the interference of organic particles, and the micro-plastic loss is easy to occur during collection, so that the selectivity is not strong and the recovery rate is not high. In addition, the density flotation method uses a large amount of inorganic salts such as sodium chloride, calcium chloride, magnesium chloride and the like, so that reagent waste and environmental pollution are caused.
The method for treating the liquid sample by the wet digestion method mainly comprises the following steps: strong base digestion, strong acid digestion, hydrogen peroxide digestion, a mixed digestion method and the like, wherein the loss of the micro-plastic is easily caused by the strong base digestion and the strong acid digestion, and the hydrogen peroxide digestion is relatively mild. The pretreatment method should select proper digestion reagent, digestion temperature and digestion time to maximally remove interfering substances while ensuring that micro-plastics are not lost. The application number is CN202110681624.4, and the name is 'a method for quantitatively analyzing micro-plastics in leaf vegetables', a sample is digested by using nitric acid and hydrogen peroxide, and the polystyrene micro-plastics are quantitatively detected. It should be noted that a large amount of oxidative and corrosive digestion liquid residues exist in the solution after wet digestion, the filter membrane is easy to corrode during filtration, so that the pore diameter of the surface of the filter membrane is changed, particulate matters in the test solution are gathered at the position where the pore diameter of the filter membrane is increased, and the corrosion product of the filter membrane is easy to block the filter membrane.
At present, the method for pretreating the micro-plastic in the liquid sample mainly has the following common problems: 1. the micro-plastics in the liquid sample are easy to agglomerate, and the micro-plastics are unevenly distributed on the surface of the filter membrane after being filtered and enriched; 2. the density flotation method can not eliminate the interference of organic particles, the recovery rate is lower than 50 percent, and even lower than 30 percent when the interference is serious; 3. the residual digestion liquid after wet digestion corrodes the filter membrane, which affects the filtration and enrichment effects. The same problem occurs with polyethylene microplastics in liquid samples when the above pretreatment method is used.
Disclosure of Invention
The invention aims to provide a pretreatment method for detecting polyethylene micro-plastic in a liquid sample, which is used for eliminating the interference of organic particles in the pretreatment process of the polyethylene micro-plastic, improving the recovery rate and avoiding the influence of the corrosion of a filter membrane on the counting of the sample during the filtration.
The invention provides the following technical scheme:
after a liquid sample is digested into a clear digestion solution by using a hydrogen peroxide solution, adding sodium bicarbonate to remove excessive hydrogen peroxide in the digestion solution in a heating and ultrasonic mode, adding ethanol into the digestion solution, and dispersing agglomerated polyethylene micro-plastics in the digestion solution.
Preferably, the hydrogen peroxide solution is added to the liquid sample in an amount of: the volume ratio of the hydrogen peroxide solution to the liquid sample is 1: 1-4, wherein the mass percentage of the hydrogen peroxide in the hydrogen peroxide solution is 30%.
Preferably, the digestion time of the hydrogen peroxide solution on the liquid sample is 12-36h, and the digestion temperature is 40-55 ℃.
Preferably, the concentration of sodium bicarbonate in the digestion solution after the addition of sodium bicarbonate is 3.5-5.0 g/L.
Preferably, the digestion solution is heated to 40-55 ℃ after adding sodium bicarbonate.
Preferably, after the digestion solution is added with sodium bicarbonate, the solution is subjected to ultrasonic treatment for 3 to 8 hours.
Preferably, the digestion solution is prepared by mixing ethanol and the digestion solution according to the volume ratio of 1: 3-4, adding ethanol, and dispersing the polyethylene micro plastic.
Preferably, the ethanol is chromatographically pure ethanol.
Preferably, the digestion solution uniformly dispersed with ethanol is filtered by a filter membrane, and polyethylene micro plastic is uniformly enriched on the filter membrane.
The pretreatment method is applied to detection of polyethylene micro-plastics in a coating, or detection of polyethylene micro-plastics absorbed into organisms, or detection of polyethylene micro-plastics in blood.
The invention has the beneficial effects that:
according to the invention, after a liquid sample is digested into a clear solution by using a hydrogen peroxide solution, sodium bicarbonate is added to reach a proper concentration, and excessive hydrogen peroxide in a system is removed by ultrasound, so that the interference of organic particles can be eliminated without changing the appearance and molecular structure of the polyethylene micro-plastic, and the polyethylene micro-plastic is stable under the digestion condition; after excessive hydrogen peroxide in the solution is removed, the filter membrane is not corroded in the subsequent filtration process, so that the performance of the filter membrane is kept, and the micro plastic cannot penetrate through the filter membrane and can not be accumulated on the filter membrane.
Because the polyethylene micro-plastics in the liquid sample are easy to agglomerate due to hydrophobicity, a proper amount of ethanol is added into the solution for dispersion, so that the polyethylene micro-plastics on the filter membrane are uniformly dispersed and convenient to count.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic process flow diagram of the present invention;
FIG. 2 is a morphology of polyethylene micro-plastic under a scanning electron microscope before digestion of a liquid sample according to the present invention;
FIG. 3 is a Raman spectrum of a liquid sample of the present invention before digestion of the polyethylene microplastic;
FIG. 4 is a morphology of a polyethylene micro-plastic under a scanning electron microscope after digestion of a liquid sample according to example 1 of the present invention;
FIG. 5 is a Raman spectrum of a polyethylene micro-plastic after digestion of a liquid sample according to example 1 of the present invention;
FIG. 6 is a scanning electron micrograph of the effect of excess hydrogen peroxide in the digestion solution on the silver filter without sodium bicarbonate removal;
FIG. 7 is a scanning electron micrograph of the effect of excess hydrogen peroxide in the digestion solution on the silver filter membrane eliminated by sodium bicarbonate;
FIG. 8 is a micro-Raman topography of the polyethylene micro-plastic of the target in example 1;
FIG. 9 is a Raman spectrum of the polyethylene micro-plastic as the target in example 1;
FIG. 10 is a micro-Raman micrograph of polyethylene microplastics in alveolar lavage fluid from example 2;
FIG. 11 is a Raman spectrum of polyethylene microplastic in alveolar lavage fluid from example 2;
FIG. 12 is a photograph of the layered agglomeration of polyethylene micro-plastics in a liquid sample without dispersion treatment;
FIG. 13 is a photograph showing that the polyethylene microplastic subjected to the ethanol dispersion treatment is uniformly distributed in the liquid sample.
Detailed Description
The main reagents and instruments used in the following examples are as follows:
(1) reagent
Polyethylene micro plastic: the particle size is 22-45 mu m, and the particles are purchased from Sigma-Aldrich company;
hydrogen peroxide (30% w/w): analytically pure, purchased from chemical reagents of national drug group, ltd;
sodium bicarbonate: analytically pure, purchased from chemical reagents of national drug group, ltd;
ethanol: chromatographically pure, available from merck, germany.
(2) Laboratory apparatus
inVia type micro raman, manufacturer: renishaw;
quanta650 type scanning electron microscope, manufacturer: FEI;
e180h model constant temperature ultrasonic cleaning apparatus, manufacturer: elma.
The pretreatment method for detecting the polyethylene micro-plastic in the liquid sample, disclosed by the invention, has the process flow chart shown in figure 1, and comprises the following steps of:
s1, taking a liquid sample with a certain volume, digesting the liquid sample into a clear digestion solution by using a hydrogen peroxide solution, wherein a large amount of hydrogen peroxide exists in the liquid sample;
s2, adding sodium bicarbonate, removing excessive hydrogen peroxide in the digestion solution in a heating and ultrasonic mode, heating to 40-55 ℃, and performing ultrasonic treatment for 3-8h, wherein no bubbles appear in the solution to indicate that the hydrogen peroxide is completely decomposed; after adding sodium bicarbonate, the concentration of the sodium bicarbonate in the digestion solution is 3.5-5.0 g/L;
and S3, adding ethanol into the digestion solution, and dispersing the agglomerated polyethylene micro-plastic in the digestion solution.
Wherein, the adding amount of the hydrogen peroxide solution in the liquid sample is as follows: the volume ratio of the hydrogen peroxide solution to the liquid sample is 1: 1-4, wherein the mass percentage of the hydrogen peroxide in the hydrogen peroxide solution is 30%.
The digestion time of the hydrogen peroxide solution to the liquid sample is 12-36h, and the digestion temperature is 40-55 ℃.
And (3) dissolving the digestion solution in a volume ratio of ethanol to the digestion solution of 1: 3-4, adding ethanol, and dispersing the polyethylene micro plastic.
The liquid sample treated by the method can be further filtered, and the polyethylene micro-plastic can be uniformly enriched on the filter membrane for qualitative and quantitative analysis of microscopic counting.
Example 1
Taking the inner coating of a paper cup for disposable drinking in the market as an example, the inner coating of the paper cup is mostly made of polyethylene, and the polyethylene coating can partially fall off under the condition of high temperature or mechanical extrusion to generate polyethylene micro plastic which enters the human body when drinking water. In order to show the characteristics of the invention, 3 disposable drinking paper cups with polyethylene films as inner coatings are taken, 150mL of pure water with the temperature of 100 ℃ is added, and 20mL of pure water is taken out for testing after 10 min. Adding 6mL of hydrogen peroxide (30% w/w) into 20mL of test solution, digesting for 12h at 40 ℃, adding 130mg of sodium bicarbonate after digestion, shaking up, carrying out ultrasonic reaction for 3h at 40 ℃, adding 6.5mL of ethanol after no bubbles emerge, and mixing uniformly, thereby completing the pretreatment step.
In order to show the effectiveness of the invention, a silver filter membrane with the aperture of 1.0 μm is used for filtration, the particles on the silver filter membrane are observed and identified under the micro-Raman, Raman spectrum analysis is carried out on all the particles under the resolution which can be achieved by an instrument, the Raman spectrum is shown in figure 5, the result shows that 43% of the particles on the filter membrane are polyethylene micro-plastics, one PE micro-plastic in a sample is shown in figure 8, and the corresponding Raman spectrum of the polyethylene micro-plastic is shown in figure 9. In addition, the above 3 paper cup samples were subjected to a polyethylene micro-plastic labeling experiment, and the counting results of the labeling experiment showed an average recovery rate of 94% using the pretreatment method of the present invention.
The labeling experiment was as follows:
preparation and detection of reference samples: and (3) marking 100 mu L of polyethylene micro-plastic suspension, adding the polyethylene micro-plastic suspension into 20mL of pure water, directly filtering without pretreatment, cutting, preparing and loading, and counting as a reference. The measuring instrument uses micro-Raman, takes 20 fields for observation under 100 times, and calculates the total number of the observed polyethylene micro-plastics; 3 samples were prepared.
Preparation and detection of the original sample: the disposable drinking paper cup with polyethylene film as the inner coating was taken 3, 150mL of pure water at 100 ℃ was added, 20mL of sample was taken, and the preparation was carried out on the cup by filtration and cutting after the pretreatment in example 1. Using micro-Raman, 20 fields are taken at 100 times for observation, and the total number of the polyethylene micro-plastics observed is calculated; 3 original samples were prepared.
Preparation of a labeled sample: and adding 100 mu L of polyethylene micro-plastic suspension into 20mL of sample, performing pretreatment, filtering, cutting and preparing the upper machine. The measuring instrument uses micro-Raman, takes 20 fields for observation under 100 times, and calculates the total number of the observed polyethylene micro-plastics; 3 spiked samples were prepared.
The recovery data are shown in Table 1. The original sample adding mark counting value and the original sample counting value have no corresponding relation, and the heterogeneous experiment can not realize similar correspondence, although 100 mu L is absorbed, the particles which can be counted in the 100 mu L are not constant. But the number averaged over multiple measurements is accurate and comparable.
Table 1 recovery of example 1
Example 2
The micro-plastics can enter the organism by means of air inhalation, mainly deposit in the lungs, and further create health risks. The micro-plastic inhalation can be evaluated by studying the particle size and content of the micro-plastic in the alveolar lavage fluid. Collecting 1mL of experimental rat alveolar lavage fluid sucked with polyethylene micro-plastic, diluting the solution to 5mL with pure water, adding 2.0mL of hydrogen peroxide (30% w/w), digesting the solution at 45 ℃ for 24h, adding 28mg of sodium bicarbonate after digestion, shaking the solution evenly, ultrasonically reacting the solution at 45 ℃ for 4h, adding 2mL of ethanol after no bubbles emerge, and uniformly mixing the solution, thereby completing the pretreatment step of the invention. To demonstrate the effectiveness of the present invention, subsequent filtration with a silver filter membrane of 1.0 μm pore size was performed, and the particles on the silver filter membrane were observed under microscopic Raman and characterized, as shown in FIG. 10, and polyethylene microplastics in alveolar lavage fluid were found experimentally, and the Raman spectrum of the corresponding polyethylene microplastics is shown in FIG. 11. In addition, 3 experimental rats which are not inhaled with the polyethylene micro-plastic are respectively taken to carry out an in-vitro labeling experiment of the polyethylene micro-plastic by taking 1mL of alveolar lavage fluid, and the counting result of the labeling experiment shows that the average recovery rate of the pretreatment method is 96 percent.
The labeling experiment was as follows:
preparation and detection of reference samples: the results of example 1 were used.
Preparation and detection of the original sample: a1 mL sample of alveolar lavage fluid was collected as described in example 2, pretreated, filtered, and cut to prepare a machine. Microscopic raman was used for the measurement instrument, and 20 fields of view were taken at 100 x, and the total number of polyethylene microplastics observed was calculated. 3 original samples were prepared.
Preparation of a labeled sample: and adding 100 mu L of polyethylene micro-plastic suspension into 1mL of sample, performing pretreatment, filtering, cutting and preparing the upper machine. Microscopic raman was used for the measurement instrument, and 20 fields of view were taken at 100 x, and the total number of polyethylene microplastics observed was calculated. 3 spiked samples were prepared.
The recovery data are shown in Table 2.
Table 2 recovery of example 2
Example 3
The presence of the microplastic in a living body can be evaluated by detecting the microplastic in a blood sample, and a general microplastic has an average particle size of about 20 μm or more, and is hardly taken into blood by organ filtration after being inhaled into a alveolar. Collecting 1mL of blood sucked into a polyethylene micro-plastic experimental rat, diluting the blood to 5mL by using pure water, adding 4mL of hydrogen peroxide (30% w/w), digesting the blood at 55 ℃ for 36h to obtain a yellowish clear solution, adding 35mg of sodium bicarbonate after digestion, shaking the solution uniformly, carrying out ultrasonic reaction at 55 ℃ for 8h, adding 3mL of ethanol after no bubbles emerge, and mixing the ethanol uniformly to complete the pretreatment step. To demonstrate the effectiveness of the present invention, a silver filter with a pore size of 1.0 μm was subsequently used for filtration, and the particles on the silver filter were observed under micro-raman and characterized, and polyethylene micro-plastics were not found in the blood sample in the experiment. In addition, 3 experimental rats which are not inhaled with the polyethylene micro-plastic are respectively taken 1mL of blood to carry out an in-vitro polyethylene micro-plastic labeling experiment, and the counting result of the labeling experiment shows that the average recovery rate of the pretreatment method is 90 percent.
The labeling experiment was as follows:
preparation and detection of reference samples: the results of example 1 were used.
Preparation and detection of the original sample: a blood sample (1 mL) was taken according to the procedure in example 3, pretreated, filtered and cut to prepare a machine. Microscopic raman was used for the measurement instrument, and 20 fields of view were taken at 100 x, and the total number of polyethylene microplastics observed was calculated. 3 original samples were prepared.
Preparation of a labeled sample: and adding 100uL of polyethylene micro-plastic suspension into 1mL of sample, performing pretreatment, filtering, cutting and preparing the upper machine. Microscopic raman was used for the measurement instrument, and 20 fields of view were taken at 100 x, and the total number of polyethylene microplastics observed was calculated. 3 spiked samples were prepared.
The recovery data are shown in Table 3.
Table 3 recovery of example 3
Generally, a plurality of oxidative digestion modes can cause the degradation of the micro plastic, and the degradation is divided into two conditions, namely, the shape is changed, if the shape is irregular, edges and corners are rounded and not formed, or the original particle size is larger, the particles are broken in the degradation process and are changed into a plurality of fine particles; secondly, the chemical groups on the surface are changed, such as the main functional groups disappear or new functional groups are added after the surface is oxidized, so that the Raman spectrum is changed. The present invention solves the problem, and fig. 2 to 5 show the morphology of the polyethylene micro plastic particles before and after digestion of the liquid sample of example 1 of the present invention and the raman spectrum of the polyethylene micro plastic, and as can be seen from the graphs, the morphology of the polyethylene micro plastic and the functional groups on the surface of the polyethylene micro plastic are not significantly changed, which means that the digestion mode is suitable for the pretreatment of the polyethylene micro plastic.
After the digestion step of the invention, a large amount of hydrogen peroxide exists in the system, and the system is an oxidizing system. The former method directly uses a filter membrane for filtration, but the residual hydrogen peroxide in the system can destroy the filter membrane to different degrees during filtration (as shown in figure 6), and the destruction is divided into two principles, namely, the oxidation of the hydrogen peroxide can oxidize the fiber filter membrane to denature the surface and the interior of the fiber filter membrane; secondly, the metal filter membrane such as iron and silver filter membrane can catalyze the decomposition of hydrogen peroxide, and the surface structure of the metal filter membrane can be changed while the hydrogen peroxide is decomposed, as shown in fig. 6, the small particles which can be intercepted originally penetrate through the filter membrane, and the micro-plastic which is distributed on the filter membrane uniformly can be enriched at the most easily passing place because of the non-uniform surface of the filter membrane during the filtration, so that the micro-plastic is enriched on the surface unevenly, and the counting is influenced greatly. In addition, the filter membrane can fall off into the digestion solution to cause pollution after being subjected to oxidation or catalysis.
As shown in FIG. 7, in the examples 1-3 of the present invention, excess hydrogen peroxide in the digestion solution is eliminated by sodium bicarbonate, and after the sample is filtered by the filter membrane, the surface of the filter membrane is intact, the structure is not damaged, and the polyethylene micro plastic filtration and the uniform distribution on the filter membrane are not affected.
As shown in fig. 12, it is found by visual observation in the digestion solution that polyethylene particle standard is used, and in the sample which is not subjected to the ethanol dispersion treatment, polyethylene micro plastic particles float on the liquid surface and are agglomerated and layered, and the layering phenomenon means that the polyethylene micro plastic particles are agglomerated during filtration, and finally cause non-uniformity on the filter membrane, which is a phenomenon to be avoided. As shown in FIG. 13, the sample subjected to ethanol dispersion treatment is used, the polyethylene micro-plastics are uniformly dispersed in the whole digestion solution, the dispersion state is stable for at least 1h, the effect is good, and the polyethylene micro-plastics are uniformly distributed on the filter membrane during filtration, so that the counting is convenient.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The pretreatment method for detecting the polyethylene micro-plastic in the liquid sample is characterized in that after the liquid sample is digested into a clear digestion solution by using a hydrogen peroxide solution, sodium bicarbonate is added to remove excessive hydrogen peroxide in the digestion solution in a heating and ultrasonic mode, ethanol is added into the digestion solution, and the agglomerated polyethylene micro-plastic in the digestion solution is dispersed.
2. The pretreatment method according to claim 1, wherein the hydrogen peroxide solution is added to the liquid sample in an amount of: the volume ratio of the hydrogen peroxide solution to the liquid sample is 1: 1-4, wherein the mass percentage of the hydrogen peroxide in the hydrogen peroxide solution is 30%.
3. The pretreatment method according to claim 2, wherein the digestion time of the liquid sample with the hydrogen peroxide solution is 12 to 36 hours, and the digestion temperature is 40 to 55 ℃.
4. The pretreatment method according to claim 3, wherein the concentration of sodium bicarbonate in the digestion solution after addition of sodium bicarbonate is 3.5 to 5.0 g/L.
5. The pretreatment method according to claim 3, wherein the digestion solution is heated to 40 to 55 ℃ after adding sodium hydrogencarbonate.
6. The pretreatment method according to claim 3, wherein the digestion solution is subjected to ultrasonic treatment for 3 to 8 hours after the addition of sodium bicarbonate.
7. The pretreatment method according to claim 3, wherein the digestion solution is prepared by mixing ethanol and the digestion solution in a volume ratio of 1: 3-4, adding ethanol to disperse the polyethylene micro-plastic.
8. The pretreatment method according to claim 7, wherein the ethanol is chromatographically pure ethanol.
9. The pretreatment method according to claim 3, wherein the digestion solution uniformly dispersed with ethanol is filtered through a filter membrane, and the polyethylene micro plastic is uniformly concentrated on the filter membrane.
10. Use of the pretreatment method of any one of claims 1 to 9 for detecting polyethylene microplastics in a coating, or for detecting the inhalation of polyethylene microplastics into a living organism, or for detecting polyethylene microplastics in blood.
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108181154A (en) * | 2017-11-23 | 2018-06-19 | 广东海洋大学 | The detection method of micro- plastics in a kind of organism |
| WO2018140995A1 (en) * | 2017-01-31 | 2018-08-09 | Technische Universität Wien | Method for determining the plastic content in water samples and in waste water samples |
| CN110108629A (en) * | 2019-06-12 | 2019-08-09 | 深圳市美信分析技术有限公司 | The detection method of micro- plastic grain in a kind of chemical product |
| CN110646334A (en) * | 2019-09-29 | 2020-01-03 | 华东理工大学 | Rapid analysis method for small-size micro-plastic in water sample |
| CN111398003A (en) * | 2020-04-30 | 2020-07-10 | 山东省科学院海洋仪器仪表研究所 | Digestion solution for digesting organic impurities in micro-plastic, preparation method thereof and digestion method based on digestion solution |
| CN111474132A (en) * | 2020-03-31 | 2020-07-31 | 浙江省海洋水产研究所 | Rapid detection method for content of micro-plastic in water body and application |
| CN112005094A (en) * | 2018-03-07 | 2020-11-27 | 玛格丽特·安娜·莱蒂齐娅·费兰特 | Method for extracting and measuring micro-plastics in sample containing organic and inorganic matrix |
| CN113474301A (en) * | 2019-02-18 | 2021-10-01 | 凯米拉公司 | Method for evaluating and optionally selecting suitable chemicals for removing micro-plastics in a liquid matrix |
| CN113474302A (en) * | 2019-02-18 | 2021-10-01 | 凯米拉公司 | Method for monitoring and optionally controlling the removal of microplastics from water containing microplastics |
-
2021
- 2021-12-27 CN CN202111618321.4A patent/CN114486476A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018140995A1 (en) * | 2017-01-31 | 2018-08-09 | Technische Universität Wien | Method for determining the plastic content in water samples and in waste water samples |
| CN108181154A (en) * | 2017-11-23 | 2018-06-19 | 广东海洋大学 | The detection method of micro- plastics in a kind of organism |
| CN112005094A (en) * | 2018-03-07 | 2020-11-27 | 玛格丽特·安娜·莱蒂齐娅·费兰特 | Method for extracting and measuring micro-plastics in sample containing organic and inorganic matrix |
| CN113474301A (en) * | 2019-02-18 | 2021-10-01 | 凯米拉公司 | Method for evaluating and optionally selecting suitable chemicals for removing micro-plastics in a liquid matrix |
| CN113474302A (en) * | 2019-02-18 | 2021-10-01 | 凯米拉公司 | Method for monitoring and optionally controlling the removal of microplastics from water containing microplastics |
| CN110108629A (en) * | 2019-06-12 | 2019-08-09 | 深圳市美信分析技术有限公司 | The detection method of micro- plastic grain in a kind of chemical product |
| CN110646334A (en) * | 2019-09-29 | 2020-01-03 | 华东理工大学 | Rapid analysis method for small-size micro-plastic in water sample |
| CN111474132A (en) * | 2020-03-31 | 2020-07-31 | 浙江省海洋水产研究所 | Rapid detection method for content of micro-plastic in water body and application |
| CN111398003A (en) * | 2020-04-30 | 2020-07-10 | 山东省科学院海洋仪器仪表研究所 | Digestion solution for digesting organic impurities in micro-plastic, preparation method thereof and digestion method based on digestion solution |
Non-Patent Citations (3)
| Title |
|---|
| 曹浩然: "催化超声去除水样残留过氧化氢的条件和动力学探究", 中国优秀硕士论文全文数据库, no. 3 * |
| 李珊 等: ""红外显微光谱法测定生活饮用水中微塑料"", 《净水技术》, vol. 40, no. 1, pages 44 - 48 * |
| 陈勇军: "金属有机骨架材料在废塑料处理方面的应用探索", 中国优秀硕士论文全文数据库, no. 3, pages 72 * |
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