CN109444332B - Device for in-situ research of environment conversion of difficultly-separated graphene oxide in actual field - Google Patents
Device for in-situ research of environment conversion of difficultly-separated graphene oxide in actual field Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 89
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 88
- 238000011160 research Methods 0.000 title claims description 13
- 238000006243 chemical reaction Methods 0.000 title claims description 11
- 238000011065 in-situ storage Methods 0.000 title claims description 10
- 239000011229 interlayer Substances 0.000 claims abstract description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000000502 dialysis Methods 0.000 claims abstract description 25
- 239000012528 membrane Substances 0.000 claims abstract description 24
- 239000002086 nanomaterial Substances 0.000 claims abstract description 22
- 241000894006 Bacteria Species 0.000 claims abstract description 19
- 229920002521 macromolecule Polymers 0.000 claims abstract description 17
- 239000000126 substance Substances 0.000 claims description 14
- 238000004458 analytical method Methods 0.000 claims description 10
- 230000007613 environmental effect Effects 0.000 claims description 8
- 150000003384 small molecules Chemical class 0.000 claims description 6
- -1 polytetrafluoroethylene Polymers 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 4
- 239000002689 soil Substances 0.000 claims description 4
- 230000005484 gravity Effects 0.000 claims description 3
- 239000013618 particulate matter Substances 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims description 3
- 230000005068 transpiration Effects 0.000 claims description 3
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 2
- 229920000570 polyether Polymers 0.000 claims description 2
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical compound Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 claims 1
- 239000012466 permeate Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 5
- 239000002105 nanoparticle Substances 0.000 abstract description 4
- 238000002474 experimental method Methods 0.000 abstract 1
- 238000002441 X-ray diffraction Methods 0.000 description 9
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- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 description 4
- 239000002131 composite material Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000004108 freeze drying Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000008213 purified water Substances 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- XOJVVFBFDXDTEG-UHFFFAOYSA-N Norphytane Natural products CC(C)CCCC(C)CCCC(C)CCCC(C)C XOJVVFBFDXDTEG-UHFFFAOYSA-N 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- LOGSONSNCYTHPS-UHFFFAOYSA-N cyclopentane-1,3-dione Chemical compound O=C1CCC(=O)C1 LOGSONSNCYTHPS-UHFFFAOYSA-N 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- 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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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N23/207—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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Abstract
The device can simultaneously analyze the influence of bacteria, biological macromolecules and micromolecules in a water body on nano particles, comprises two acrylic plates, nine circular areas are arranged on the acrylic plates, water permeable hole groups are respectively arranged in each area, an interlayer is clamped between the two acrylic plates and the corresponding position of each circular area water permeable hole group, three groups of interlayers in each row from left to right are respectively an interlayer filter paper, a filter membrane interlayer and a dialysis bag interlayer, and screw holes are formed in four corners of each acrylic plate and are fixed by screws; the interlayer is sandwiched with the nano material graphene oxide to be analyzed. Compared with the prior art, the method can simultaneously analyze the influence of bacteria, biological macromolecules and micromolecules on the nano particles in the actual field, set a parallel experiment group and solve the problem that the nano materials in the actual field are difficult to recover.
Description
Technical Field
The invention relates to an analysis device for interaction between graphene oxide and actual site substances, in particular to a device capable of analyzing influence of bacteria, biological macromolecules and micromolecules in an actual site on the graphene oxide at the same time, and belongs to the technical field of environmental ecological safety.
Background
With the wide application of nano materials, the release of nano materials in the environment is inevitable. Research by many scholars has demonstrated the widespread existence of nanomaterials, especially artificial nanomaterials, in water bodies. Therefore, research on the single and composite influence of bacteria, biological macromolecules and small molecules on nano materials in an actual field is necessary. The traditional research device can only simulate the actual environment through a laboratory to research single factors, and is difficult to simultaneously analyze the influence of bacteria, biological macromolecules and micromolecules on the nanometer material in the actual field. Also, there is a difficulty in separating the nanomaterial in the actual field.
Therefore, it is necessary to design a device for in situ research of environmental conversion of graphene oxide difficult to separate in a practical field.
Disclosure of Invention
The invention aims to solve the problems that the traditional research device can not simultaneously analyze the influence of bacteria, biological macromolecules and micromolecules on nano materials, can not be applied to natural environment and can not easily separate the nano materials in an actual field.
Technical scheme of the invention
The device can simultaneously analyze the influence of bacteria, biomacromolecules and micromolecules on nano particles in an actual field, mainly comprises two acrylic (PC) plates, screw holes are formed in four corners of the two acrylic plates and are fixed through screws, nine circular areas are formed in the acrylic plates, water permeable hole groups are respectively formed in each area, one of a filter paper interlayer, a filter membrane interlayer or a dialysis bag interlayer is clamped between the two acrylic plates and the positions corresponding to the water permeable hole groups of the circular areas, and nano material graphene oxide is respectively placed in the middle of each interlayer; when the analysis device is placed in a water body of an actual field, water containing various substances respectively enters the device from top to bottom along with the gravity and the transpiration; because the filter paper can block particles, the graphene oxide in the interlayer of the filter paper can react with bacteria, biological macromolecules and micromolecules in water; the filter membrane can block particles and bacteria, so that the graphene oxide in the filter membrane interlayer can react with biological macromolecules and micromolecules in water; because the dialysis bag can block particulate matter, bacterium and biological macromolecule, consequently the oxidation graphite alkene in the dialysis bag intermediate layer can only with the biological micromolecule effect in the aquatic.
The acrylic plate is a two-layer acrylic thin plate with holes and the thickness of the two-layer acrylic thin plate is 2mm, and the shape of the acrylic thin plate is any geometric shape including but not limited to square, rectangle, rhombus, circle or ellipse. The sandwich structure is double-layer filter paper (or filter membrane or dialysis bag) with nano material graphene oxide sandwiched in the middle. The interlayers refer to the placing sequence, and three groups of the interlayers in each row from left to right are the same and are respectively filter paper interlayers, filter membrane interlayers or dialysis bag interlayers.
The filter paper is made of polytetrafluoroethylene with the aperture of 0.45 mu m, the aperture capable of intercepting the oxidized graphene is selected in consideration of the sheet diameter of the selected oxidized graphene being 500nm-5 mu m, and meanwhile, the polytetrafluoroethylene capable of existing for a long time is selected in consideration of the time durability of the device in the research process. The filter membrane is a polyether brave water system filter membrane with a pore size of 0.45 μm. The dialysis bag is a dialysis bag with molecular weight cutoff of 3500D.
Besides being applied to water, the device can also be applied to soil and other nano materials, and can recover the nano materials difficult to separate.
The invention has the advantages and beneficial effects that:
(1) the analysis device can simultaneously analyze the influence of bacteria, biological macromolecules and small molecules on the nano particles in an actual field; (2) the analysis device is suitable for analyzing the interaction between various nano materials and an actual field; (3) the analysis device is suitable for natural environment soil and laboratory simulation soil environment; (4) the analysis device can be used for even 3 groups of parallel tests; (5) the analysis device solves the problem that graphene oxide is difficult to recover in an actual field
Drawings
FIG. 1 is a schematic front view of the apparatus of the present invention.
Fig. 2 is an isometric view of the device of the present invention.
Figure 3 is a TEM image of graphene oxide after 2 d.
Fig. 4 is a TEM image of graphene oxide after 7 d.
FIG. 5 is a comparison of Fourier infrared spectra of graphene oxide after 2d for three different cases.
FIG. 6 is a comparison of Fourier infrared spectra of graphene oxide after 7d for three different cases.
Fig. 7 is an X-ray diffraction pattern of pristine graphene oxide.
FIG. 8 is an XRD spectrum of graphene oxide under filter paper conditions; wherein A is data after 2d, and B is data after 7 d.
FIG. 9 is an XRD (X-ray diffraction) spectrum of graphene oxide under the condition of a filter membrane; wherein A is data after 2d, and B is data after 7 d.
FIG. 10 is an XRD pattern of graphene oxide under dialysis bag conditions; wherein A is data after 2d, and B is data after 7 d.
In the figure: 1 acrylic plate, 2 screw holes, 3 hole groups of permeating water, 4 dialysis bag interlayers containing nano material graphene oxide, 5 filter membrane interlayers containing nano material graphene oxide, and 6 filter paper interlayers containing nano material graphene oxide.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings.
Referring to fig. 1 and 2, the device for in-situ research of environment conversion of graphene oxide difficult to separate in an actual field can simultaneously analyze the influence of bacteria, biological macromolecules and small molecules on the graphene oxide in the actual field, and comprises two square acrylic plates 1, wherein screw holes 2 are formed in four corners of the two acrylic plates 1 and are fixed through screws, nine circular areas are formed in each acrylic plate, and a water permeable hole group 3 is formed in each area. An interlayer containing nano-material graphene oxide is clamped between the two acrylic plates 1 and at the position corresponding to the region where the water-permeable hole group of each circular region is located, the interlayer is one of a filter paper interlayer 6, a filter membrane interlayer 5 or a dialysis bag interlayer 4, the interlayer reference placing sequence is that three groups in each row from left to right are the same, and the three groups are respectively the filter paper interlayer 6, the filter membrane interlayer 5 or the dialysis bag interlayer 4. And the nano material graphene oxide is respectively placed between the two films of each interlayer. When the analysis device is placed in the water body of an actual field, water containing various substances enters the device from top to bottom along with gravity and transpiration respectively. Because the filter paper can block particulate matters, the graphene oxide in the filter paper interlayer 6 can perform a composite action with bacteria, biological macromolecules and small molecules in water. Because the filter membrane can block particulate matters and bacteria, the graphene oxide in the filter membrane interlayer 5 can have a composite effect with biological macromolecules and small molecules in water. Because the dialysis bag can block particulate matter, bacterium and biological macromolecule, consequently the oxidation graphite alkene in dialysis bag intermediate layer 4 can only with the biological micromolecule effect in the water.
A device for in-situ research of environment conversion of graphene oxide difficult to separate in an actual field comprises the following specific operation steps: weighing 25mg of flake graphene oxide, dispersing the flake graphene oxide in purified water, ultrasonically dispersing for 4h, performing suction filtration on filter paper, a filter membrane and a dialysis bag, filling an interlayer material into a device, putting the device into a water body to be analyzed, taking out the device after 2d, dismantling an acrylic plate structure, eluting the graphene oxide, freeze-drying the graphene oxide, grinding the graphene oxide into powder, and characterizing the graphene oxide.
The above is the first set of samples.
And (3) comparison test:
the second set of samples:
weighing 25mg of flake graphene oxide, dispersing the flake graphene oxide in purified water, ultrasonically dispersing for 4h, performing suction filtration on the surfaces of filter paper, a filter membrane and a dialysis bag, filling an interlayer material into a device, putting the device into a water body, taking out the device after 7d, dismantling an acrylic plate structure, eluting the graphene oxide, freeze-drying the graphene oxide, grinding the graphene oxide into powder, and characterizing the graphene oxide.
Third set of samples:
raw graphene oxide was used as a control.
Measuring polycyclic aromatic hydrocarbon by an Agilent gas chromatograph-mass spectrometer, performing spectrum library analysis, and bombarding an ion source (EI) by electrons, wherein the temperature of the ion source is 230 ℃; the temperature of the four-level bar is 150 ℃; the temperature of a front sample inlet is 300 ℃; the Aux-2 temperature is 300 ℃, and the solvent delay time is 4.5 min; the measurement is performed by selecting a full scan mode.
The main result is shown in the following table, compared with original graphene oxide, basically, the peaks of polycyclic aromatic hydrocarbons in graphene oxide mostly exist in 2d and 7d later graphene oxide, but the peak area (content) is obviously increased compared with the original graphene oxide, which indicates that the graphene oxide is placed in the device and obviously adsorbs organic matters in water, and the data amount after the obvious 7d is greater than the data after 2d, which indicates that the adsorbed organic matters are more and the possible species are also gradually enriched along with the increase of time under the general condition. Meanwhile, some substances are such as: 1,3-Cyclopentanedione and the like, which can be detected in original graphene oxide but does not exist in the graphene oxide after being treated by the device, and may be environmental conversion occurring in the experimental process or not extracted in the extraction process.
TABLE 1
And (3) eluting graphene oxide in the device, freeze-drying, ultrasonically dispersing in an ethanol solution to make the concentration of the graphene oxide be 10mg/L, adding 1 drop of graphene oxide onto the ultrathin carbon film, and determining by using a transmission electron microscope. As can be seen from fig. 3 and 4, after 7d (fig. 4), graphene oxide was more significantly laminated than after 2d (fig. 3), and the impurities were more on the surface.
Drying a small amount of graphene oxide powder and potassium bromide solid, and measuring an infrared spectrogram by a potassium bromide tabletting method, wherein the scanning range is 400-4000cm-1As can be seen from fig. 5 and 6, the difference between the graphene oxide after 2d (fig. 5) and the graphene oxide after 7d (fig. 7) is 2300cm, which is more remarkable than the original graphene oxide-1The peak is aromatic, the intensity of the peak increases gradually with time, and the substance exists but is not prominent compared with the original graphene oxide. 3600cm-1The peak is highlighted in the data after 7d, the peak is a-OH stretching vibration peak which can be used as a standard for judging whether alcohols, phenols and organic acids exist, and the peak is highlighted after 7d, which shows that the-OH intensity is gradually increased as the substances are obviously increased along with the increase of time.
Taking a proper amount of graphene oxide powder, placing the graphene oxide powder on a glass slide, and measuring by using an X-ray diffractometer, wherein the scanning angle is 5-90 degrees. As shown in fig. 7 to 10 (fig. 7 is an XRD pattern of original graphene oxide, fig. 8 is an XRD pattern of graphene oxide under filter paper, fig. 9 is an XRD pattern under filter membrane, and fig. 10 is an XRD pattern under dialysis bag), when 2 θ of original graphene oxide (fig. 7) is 11.38 °, weak and broad peaks are present, and when comparing the data after 2d and the data after 7d, the data after 2d shows less peaks, but the number of peaks after 7d is significantly large, mainly because the amount of adsorbed substances is large or the amount of adsorbed substances is significantly increased, the peaks are highlighted. After 2d, fig. 8 to 10 show that a peak is obvious when 2 θ is about 26 °, but the data after 7d does not show the peak, and it is known from the examination of the literature that the substance corresponding to the peak may be graphene, it is suspected that graphene oxide is reduced to graphene by a part of substances after 2d, but the peak disappears after 7d, it is suspected that the reduced graphene is not too stable, and is oxidized to graphene oxide under the action of ions in water, and the adsorbed substance and the adsorbed amount are gradually increased, and the peak is gradually increased, so that the peak of graphene is not obvious. And the graphene has narrow peaks and small interlayer spacing, and the main reason is that a large number of oxygen-containing groups are introduced to the surface and the edge of the graphene oxide in the graphene oxidation process, so that the interlayer spacing of the graphene oxide is increased. Comparing the data of the filter paper, the filter membrane and the dialysis bag, it can be seen that the peak of the 26-degree graphene gradually decreases from the filter paper, the filter membrane to the dialysis bag, and the main reason is that the degree of reduction of the graphene oxide is different due to different substances contacted by the graphene oxide.
The foregoing detailed description describes the preferred embodiments of the present invention. It will be appreciated by those of ordinary skill in the art that changes may be made to the detailed description of the invention without inventive faculty, and that the general principles of the description may be applied to other examples. Therefore, the present invention is not limited to the above-described embodiments. Modifications and improvements within the scope of the invention will occur to those skilled in the art from the detailed description of the invention and are intended to be within the scope of the invention.
Claims (5)
1. A device for in-situ research of graphene oxide environmental conversion in an actual field comprises two acrylic plates, screw holes are formed in four corners of the two acrylic plates and fixed through screws, nine circular areas are formed in the acrylic plates, water permeable hole groups are formed in the areas respectively, one of a filter paper interlayer, a filter membrane interlayer or a dialysis bag interlayer is clamped between the two acrylic plates and in the positions corresponding to the water permeable hole groups in the circular areas respectively, and nano-material graphene oxide is placed in the middle of each interlayer; wherein the filter paper is made of polytetrafluoroethylene with a pore diameter of 0.45 μm and capable of intercepting graphene oxide, the filter membrane is a polyether valia water system filter membrane with a pore diameter of 0.45 μm and capable of intercepting bacteria, and the dialysis bag is a dialysis bag with a molecular weight cut-off of 3500D and capable of allowing small-molecular substances to permeate through the dialysis bag and react with graphene oxide; when the analysis device is placed in a water body of an actual field, water containing various substances respectively enters the device from top to bottom along with the gravity and the transpiration; the filter paper can block particles, so that the graphene oxide in the interlayer of the filter paper can react with bacteria, biological macromolecules and micromolecules in water; the filter membrane can block particles and bacteria, so that graphene oxide in the filter membrane interlayer can react with biological macromolecules and small molecules in water; the dialysis bag can block particulate matter, bacteria and biological macromolecules, so that graphene oxide in the interlayer of the dialysis bag can only act with biological micromolecules in water.
2. The device for researching environmental conversion of graphene oxide in situ in a practical field according to claim 1, is characterized in that: the sheet diameter of the graphene oxide is 500nm-5 mu m.
3. The device for researching environmental conversion of graphene oxide in situ in a practical field according to claim 1, is characterized in that: the device can be applied to water or soil, and the graphene oxide nano-material which is difficult to separate and is placed between the two acrylic plates can be recycled.
4. The device for in-situ research on environmental conversion of graphene oxide in a practical field according to any one of claims 1 to 3, wherein: the acrylic plate is in any geometrical shape.
5. The device for researching environmental conversion of graphene oxide in situ in a practical field according to claim 4, is characterized in that: the acrylic plate is square, rectangular, rhombic, circular or elliptical in shape.
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| Graphene in the Aquatic Environment: Adsorption, Dispersion;Jian Zhao等;《Environmental Science & Technology》;20140814;第48卷(第17期);第9995-10009页 * |
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