IDENTIFICATION METHOD OF PLASTIC MICROPARTICLES
20230228678 · 2023-07-20
Inventors
Cpc classification
G01J3/42
PHYSICS
International classification
G01J3/42
PHYSICS
Abstract
Provided is an identification method of plastic microparticles, including: performing an infrared analysis on plastic microparticles to identify whether the plastic microparticles include polyethylene terephthalate, polyethylene, polypropylene, or nylon 66, wherein the identification is to determine whether the plastic microparticles have a characteristic peak of each plastic, and the characteristic peak is selected from signals that do not overlap and interfere with each other in the infrared spectrum signals of each plastic.
Claims
1. An identification method of plastic microparticles, comprising: performing an infrared analysis on the plastic microparticles to identify whether the plastic microparticles comprise at least one plastic selected from a group consisting of polyethylene terephthalate, polyethylene, polypropylene and nylon 66, wherein the identification is to determine whether the plastic microparticles have characteristic peaks of each of the at least one plastic, and the characteristic peaks are selected from signals that do not overlap and interfere with each other among infrared spectral signals of each of the at least one plastic.
2. The method of claim 1, wherein the characteristic peak of the polyethylene terephthalate is at 793±5 cm.sup.−1, the characteristic peaks of the polyethylene are at 1472±5 cm.sup.−1 and 1462±5 cm.sup.−1, the characteristic peak of the polypropylene is at 841±5 cm.sup.−1 and the characteristic peak of the nylon is at 3295±5 cm.sup.−1.
3. The method of claim 1, further comprising performing pre-cleaning treatment on the plastic microparticles prior to performing the infrared analysis.
4. The method of claim 3, wherein the pre-cleaning treatment comprises removing organics by Fenton reaction and rinsing the plastic microparticles with water.
5. The method of claim 1, further comprising a pellet-forming pretreatment of the plastic microparticles with potassium bromide prior to performing the infrared analysis.
6. The method of claim 1, further comprising performing a solvent extraction on the plastic microparticles prior to performing the infrared analysis.
7. The method of claim 6, wherein the solvent extraction is performed with a solvent selected from a group consisting of tetrahydrofuran, nitrobenzene, cyclohexanone, dichloromethane, trichloromethane and carbon tetrachloride.
8. The method of claim 6, further comprising forming crystals from an extract liquid obtained by the solvent extraction, and performing the infrared analysis on the crystals to further identify whether the plastic microparticles contain constituents other than the polyethylene terephthalate, polyethylene, polypropylene and nylon 66.
9. The method of claim 1, further comprising identifying whether the plastic microparticles contain polyvinyl chloride.
10. The method of claim 1, wherein a characteristic peak of the polyvinyl chloride is at 712±5 cm.sup.−1.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
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DETAILED DESCRIPTION
[0030] The embodiments of the present disclosure will be described below through specific embodiments, and those people with ordinary knowledge in the technical field can easily comprehend the scope and effect of the present disclosure based on the contents described herein. However, the specific embodiments described herein should not be construed as limiting the scope of the present disclosure. The listed technical features or solutions can be combined with each other. The present disclosure can also be implemented or applied through different embodiments. The details can also be given modifications or recombination according to different viewpoints and applications without departing from the scope and the spirit of the present disclosure.
[0031] Unless stated otherwise, the term “comprising,” “including,” “containing,” or “having” particular elements used herein means that other elements such as units, components, structures, regions, parts, devices, systems, steps, or connection associations can be also included rather than excluded.
[0032] Unless expressly stated otherwise, the singular forms “a,” “an,” and “the” also include the plural forms, and the “or” and “and/or” can be used interchangeably herein.
[0033] The value ranges recited herein are inclusive and can be combined, and any value falling into the value range recited herein can be used as the upper or lower limit to derive a subrange; for example, a range of values “250 mesh or above” should be understood to include any sub-range from a minimum value of 250 mesh or above ; for example, 250 mesh or above, 300 mesh or above, and 500 mesh or above, and etc . . . In addition, if a value range falls within each range described herein (e.g., 500 mesh falls into a range of 250 mesh or above), that is, the value should be deemed to be included in the scope of the present disclosure.
[0034] The present disclosure takes into account the lots of environmental impacts caused by the extremely large production and usage of PET, PE, PP, and NY, so it is particularly focused on identifying the constituents of PET, PE, PP and NY from unknown plastic microparticles. On the other hand, since PVC is also a widely used plastic, the present disclosure further provides an identification identification method of the constituents of PET, PE, PP, PVC and NY from unknown plastic microparticles. The present disclosure is characterized in that, unknown plastic microparticles can be identified in a single IR analysis to contain multiple plastic constituents without multiple and complicated steps of extraction and separation. The method is simple and fairly accurate.
[0035] In the field of material analysis and identification, infrared spectroscopy, such as Fourier-transform infrared spectroscopy (FTIR) is a widely used analytical technique. Different components respond differently to optical radiation due to differences in molecular structure. FTIR spectrometer establishes an infrared spectrum that corresponds to the specific component since different components have different degrees of absorption for each wavelength of infrared.
[0036] As shown in
[0037] The selection procedure of the present disclosure results in that the intensities of characteristic peaks are typically smaller than the known strongest peak. Thus, the characteristic peaks are not easy to identify when the range of the wave number set in the spectrum is broad, such as from 4000 cm.sup.−1 to 650 cm.sup.−1. There is a need to select a suitable narrower range according to the characteristic peaks, so as to improve the identification of the characteristic peaks and improve the accuracy of component identification. For example, the characteristic peaks of the PE of the present disclosure is selected as two peaks at 1472±5 cm.sup.−1 and 1462±5 cm.sup.−1, which can be clearly and accurately identified in a relatively narrow range of FTIR spectra, e.g., the characteristic peak of PE as mentioned above can be clearly seen in the range of 1550 cm.sup.−1 to 1350 cm.sup.−1.
[0038] As mentioned above, in order to identify the plastic constituents contained in the plastic microparticles, the present disclosure mixes five common plastics: PET, PE, PP, PVC and NY and form a pellet to obtain a plastic mixture, which is analyzed by using FTIR. The result is shown in
[0039] The present disclosure performs the following comparison and confirm procedures to establish an identification method of whether plastic mixture microparticle contains PET, PE, PP, and NY.
[0040] As shown in
[0041] As shown in
[0042] As shown in
[0043] As also shown in
[0044] In addition to the above-mentioned identification method of whether the plastic mixture microparticles contain plastic PET, PE, PP and NY, the present disclosure also provides a method for further identifying whether a plastic mixture microparticles contain PVC in an embodiment.
[0045] As shown in
[0046] The present disclosure finds that the signal intensities of characteristic peaks of some plastics are weak, so in an embodiment, solvent extraction is performed on the samples before an infrared analysis to extract specific plastic constituent. For example, in an embodiment, the signal intensity of the selected characteristic peak is relatively low which may be easily interfered and masked by other constituents, so plastic microparticles are first extracted with a solvent selected from a group consisting of tetrahydrofuran, nitrobenzene, cyclohexanone, dichloromethane, trichloromethane and carbon tetrachloride, and then filtered. The extracted plastic microparticles continue to the next step of an infrared analysis, whereas the extract liquid is crystallized to obtain the plastic and the plastic is identified by an infrared analysis. In an embodiment, the characteristic peak of PVC, which is at 712±5 cm.sup.−1, possess lower intensities, so the plastic mixture of mixed PET, PE, PP, PVC and NY is first extracted with tetrahydrofuran, and then the extracted plastic mixture is subjected to the next step of an infrared analysis. On the other hand, the extract liquid can go through crystallization to obtain PVC and the crystallized PVC is identified by an infrared analysis. Therefore, the present disclosure confirms that such a step of extraction of PVC in advance can be applied to the identification method of whether unknown plastic mixture microparticles contain PVC.
[0047] As mentioned above, the identification method of plastic microparticles of the present disclosure includes performing an infrared analysis on the plastic microparticles to identify whether the plastic microparticles contain a specific plastic constituent. The identification is to determine whether the plastic microparticles has characteristic peaks of each type of plastics, and the characteristic peaks are selected from the signals that do not overlap and interfere with each other in the infrared spectral signals of the respective plastics.
[0048] In an embodiment, before the infrared analysis, a step of pre-cleaning treatment may be applied on the plastic microparticles. The pre-cleaning treatment includes removing organics by Fenton reaction, and may also include rinsing the plastic microparticles with water. Pre-cleaning treatment may eliminate the interference of organics and impurities on the FTIR spectrum.
[0049] Fenton reaction conventionally uses ferrous ions (Fe.sup.2+) and hydrogen peroxide (H.sub.2O.sub.2) as reagents, wherein ferrous ions and hydrogen peroxide react in solution to produce free hydroxyl radicals (HO.sup.−) and perhydroxyl radicals (HOO.sup.−), so these free radicals can be applied to oxidatively decompose organic pollutants on plastic microparticles. Other improved technologies based on the conventional Fenton reaction, such as photo-Fenton processes, electro-Fenton process, photoelectro-Fenton, sono-Fenton process, and Fenton-like reaction of Advanced Oxidation Processes (AOPs), are also included in the pretreatment steps of the Fenton process of the present disclosure.
[0050] In an embodiment, the plastic microparticles are pretreated to form a pellet with potassium bromide before the infrared analysis. Since the dimension of the plastic microparticles remaining in the environment (e.g., water sources) are small, similar to the dimension of ground powder, and usually the amount of samples collected at one time is very limited. Therefore, a small amount of plastic microparticles can be mixed with potassium bromide (KBr) powder or be ground optionally, and the mixture is placed in a pellet press machine to make a transparent pellet under a pressurized, vacuum condition in order to facilitate the infrared analysis.
[0051] In other embodiments, other sample preparation methods for IR analysis can also be applied, for example, the Nujol method is by mixing a liquid such as paraffin oil with the sample powder and coating on a salt plate for measurement; the solution method is by dissolving the sample in a solvent and the liquid with the dissolved sample is used directly for measurement; or the thin film method is by melting or dissolving the sample in a solvent to form a thin film for measurement.
[0052] In an embodiment, the particle sizes of the plastic microparticles suitable for analysis is 250 mesh or above, 300 mesh or above, 500 mesh or above, for example, 250 mesh, 300 mesh, 400 mesh, 500 mesh, or 600 mesh.
[0053] According to the present disclosure, a simple flowchart of the identification method of plastic microparticles can be established, as shown in
[0054] The present disclosure will be described in further detail with reference to the following examples, which are by no means intended to limit the scope of the present disclosure.
EXAMPLE 1
[0055] Samples were collected from ambient surface water bodies in National Taiwan University (NTU). The samples were collected from the test water reservoir (A1) connected to the Hydrotech Research Institute, NTU, the water supply pipes (A2 and A3) connected to the reservoir, and a long and narrow ecological pool (B1) next to an experimental farmland. The samples were drawn from the water bodies with a water pump (model: SHIN KOMI 2HP) and the suspended microparticles were collected by filtration with a nylon filter with a pore size of 500 mesh (25 μm). The impurities were separated by the gravimetric method and collected in a 500 mL conical flask. The sample amounts of A1, A2, A3 and B1 were 2 mg, 4 mg, 6 mg, and 2 mg, and the concentrations in the sampling water were 8.0 ppb, 2.2 ppb, 3.0 ppb, and 1.0 ppb, respectively.
[0056] 20 mL of tetrahydrofuran was added to the conical flask and stirred for extraction, and then the solution was filtered through a 500 mesh nylon filter of a vacuum filter device, and then followed by the Fenton reaction. The Fenton reaction was carried out as follows: 5 mL of 1M ferrous sulfate and 5 mL of 0.5M, 30 wt % H.sub.2O.sub.2 solution were taken with a dropper and dropped on a nylon filter, and the Fenton reaction was repeated once again after 30 seconds of reaction. After that, the plastic microparticle sample on the nylon filter was rinsed with water, and then the plastic microparticle sample was transferred into a beaker, placed in an oven and dried at 75° C. On the other hand, the extract solution was placed in a fume hood to volatilize tetrahydrofuran for crystallization, followed by rinsing with water and drying. The obtained plastic microparticle sample was mixed with an appropriate amount of potassium bromide, and the mixture was made into a pellet by a pellet press machine for FTIR analysis.
[0057] As shown in
[0058] The results of this example showed that:
[0059] Sample A1 contains PET, PE, PP;
[0060] Sample A2 contains PET, PE, PP;
[0061] Sample A3 contains PET, PE, PP;
[0062] Sample B1 contains PE, NY;
[0063] Since the sampling areas of samples A1, A2 and A3 were the test water reservoirs and the water supply pipes that were connected to each other, the plastic microparticles have similar constituents. The sampling area of sample B1 was the long and narrow ecological pond next to the experimental farmland, so its plastic composition was significantly different from that of samples A1 to A3. Accordingly, the identification method of plastic microparticles of the present disclosure can effectively achieve the constituent identification of the unknown plastic microparticles.