CN113933261A - Method for detecting micro-plastic in sediment based on solubility parameter calculation - Google Patents
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Abstract
The invention provides a method for detecting micro-plastic in sediment based on solubility parameter calculation, which comprises the following steps: step 1: weighing a proper amount of freeze-dried sediment sample, adding the freeze-dried sediment sample into an ASE extraction pool, adding diatomite with the same volume as the sample, uniformly mixing, and performing accelerated solvent extraction according to the following conditions: extracting solvent: dichloromethane; the temperature is 180 ℃, the pressure is about 1500psi, the leaching volume is 80%, the heating is carried out for 9min, 3 static cycles are carried out, the purging time is 75s, and the standing time is1 min; step 2: concentrating the extracting solution, selecting a solvent with a larger solubility parameter difference value with the micro-plastic, adding a proper amount of the solvent into the concentrated extracting solution, and analyzing and detecting by using a Fourier transform infrared spectrometer after the micro-plastic is fully separated out. The method realizes selective precipitation of the micro-plastic by using solubility parameter difference, and detects the micro-plastic by adopting an infrared spectroscopy method, thereby establishing a novel method for quantitative analysis of the micro-plastic.
Description
Technical Field
The invention relates to the technical field of analysis and detection, in particular to a method for detecting micro-plastic in sediment based on solubility parameter calculation.
Background
Microplastics (MPs) are defined as plastic particles, chips or fibers with a size of less than 5mm, and are classified into primary and secondary Microplastics according to their origin, and the primary Microplastics are mainly manufactured in a microscale and used in the daily product industry such as cosmetics, such as personal care products (scrub, toothpaste, facial cleanser, etc.), cosmetics (eye shadow, nail polish, foundation fluid, etc.), drugs, resin particles, and the like. The secondary micro plastic is formed by decomposing large plastic blocks into smaller plastic fragments through external factors such as ultraviolet irradiation (photodegradation, embrittlement and photooxidation), weathering and corrosion. In recent years, environmental pollution by microplastics has been receiving increased attention, and microplastics have been reported to be detected in seawater, fresh water, soil, indoor dust, air, human and animal feces, and human placenta. As an important novel pollutant, the potential threat to human body, environment and ecosystem should be paid high attention.
At present, the method of density separation, which is used for suspending or floating the micro-plastics in the sediment in the supernatant solution by using a saturated salt solution (such as NaCl or NaI solution), is generally adopted for extracting the micro-plastics in the sediment, and the micro-plastics are further separated from the supernatant, but the method is not suitable for separating plastic particles with smaller particle size (< 10 mu m), and in the case of high-density micro-plastics, the micro-plastics can be settled at the bottom of the salt solution, so that a missing measurement phenomenon occurs. In addition, separation has been studied according to the physicochemical properties of the microplastic, for example, hydrophobic separation using oil or extraction using the adsorption capacity of nile red. At present, in the prior art, the sediment micro-plastic is calculated according to the quantity concentration, the quantity abundance of the micro-plastic is mainly reflected, and the quality concentration parameter is also one of the important indexes for evaluating the pollution condition of the micro-plastic. Through mass concentration measurement, the occurrence magnitude of the micro-plastic in an environmental medium can be reflected, and basic data are provided for overall evaluation and monitoring of the environmental pollution condition of the micro-plastic. In the actual sample analysis, a part of micro-plastics may be lost by using methanol for pre-cleaning, and the extract usually contains pigments and other organic impurities, which may interfere with the qualitative and quantitative analysis of the method.
Disclosure of Invention
In order to solve the problems in the prior art, the method utilizes the solubility parameter difference to separate out the micro-plastic, further obtains the micro-plastic through filtration, and subsequently detects the micro-plastic by adopting an infrared spectroscopy method, thereby establishing a novel method for the quantitative analysis of the micro-plastic.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for detecting micro-plastics in deposits based on solubility parameter calculation, comprising:
step 1: weighing a proper amount of freeze-dried sediment sample, adding the freeze-dried sediment sample into an ASE extraction pool, adding diatomite with the same volume as the sample, uniformly mixing, and performing accelerated solvent extraction according to the following conditions:
extracting solvent: dichloromethane; the temperature is 180 ℃, the pressure is 1500psi, the leaching volume is 80%, the heating is carried out for 9min, 3 static cycles are carried out, the purging time is 75s, and the standing time is1 min;
step 2: treating the extracted extract by adopting the following method: concentrating the extracting solution, calculating the solubility parameter of the micro-plastic, selecting a solvent with a larger difference value with the solubility parameter of the micro-plastic, adding a proper amount of the solvent into the concentrated extracting solution, after the micro-plastic is fully separated out, performing suction filtration by using a solvent filter, drying and weighing the filter membrane, slightly scraping the extract on the filter membrane, and analyzing and detecting by using a Fourier transform infrared spectrometer.
Further, the micro plastic is one or a mixture of more of PP, PE, PS, PC, PVC and PET 6.
Further, the solubility parameter of the mixture of the micro-plastics can be calculated by a group contribution method, and the calculation formula is as follows:
δ＝ρ·∑Fi/M
wherein, FiIs the molar attraction constant of each group in the molecule, ρ is the density of the polymer, and M is the molar mass of the polymer mer.
Further, the solvent is a mixed solution, and the solubility parameter of the mixed solution is calculated according to the following formula:
in the formula phii，δiIs the volume fraction and solubility parameter of the i-th component solvent, the sum of the volume fractions of all solvents ∑ ΦiIs 1.
Further, the mixed solution is one or a mixture of more of dichloromethane, isooctane, acetonitrile and methanol.
Further, in the step 2, the components and the approximate proportion of the micro plastic are determined according to the environmental survey result of the sample collection place.
Further, the difference between the solubility parameter of the micro-plastic and the solubility parameter of the solvent is recorded as |. DELTA. |, Δ δ | -not less than 3.
The method for detecting the micro-plastic in the sediment based on the solubility parameter calculation has the beneficial effects that:
according to the method, pollutants in the sediment are extracted (including micro plastic and other components) at high temperature and high pressure, the micro plastic is dissolved in the extract, the solubility parameters of the extract are changed by adding other solvents, so that the solubility parameters of the extract and the solubility parameters of the micro plastic are greatly different, the micro plastic is separated out, other co-extracted components are still in solution, the micro plastic is obtained by further filtering, and the micro plastic is detected by adopting a mature infrared spectroscopy subsequently.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and those skilled in the art can also obtain other drawings according to the drawings without creative efforts.
FIG. 1 is a flow chart of an extraction and analysis method of a method for detecting micro-plastics in sediments based on solubility parameter calculation according to an embodiment of the present application;
FIG. 2 is a graph showing the recovery rate of the micro-plastic in the sediment in different processing modes of the method for detecting the micro-plastic in the sediment based on the calculation of the solubility parameter according to the embodiment of the present application; wherein, (a) is directly filtered; (b) concentrating; (c) adjusting the solubility parameter of the system after concentration: (c1) separating out PP and PE micro-plastics by using acetonitrile, and separating out PS, PC, PVC and PET4 micro-plastics by using isooctane; (c2)6 kinds of micro plastics are separated out by methanol;
fig. 3 is an infrared spectrum of 6 kinds of micro-plastics in a deposit in different processing modes of a method for detecting the micro-plastics in the deposit based on solubility parameter calculation provided in an embodiment of the present application: (1) PP; (2) PE; (3) PS; (4) PC; (5) PVC; (6) PET, wherein (a) is directly suction filtered; (b) concentrating; (c) adjusting the solubility parameter of the system after concentration: (c)1) Separating out PP and PE micro-plastics by using acetonitrile, and separating out PS, PC, PVC and PET4 micro-plastics by using isooctane; (c)2)6 kinds of micro plastics are separated out by methanol;
FIG. 4 is an infrared spectrum of a mixed micro-plastic in different processing modes of a method for detecting the micro-plastic in the sediment based on the calculation of solubility parameters, provided by an embodiment of the application;
FIG. 5 is an infrared spectrum of the micro-plastic in the sediment of Huanghe Delta based on the method for detecting the micro-plastic in the sediment by calculation of solubility parameters.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The inventor of the application finds in research that: the solubility is best when the solubility parameter of the microplastic is consistent with the solubility parameter of the solvent, whereas the greater the difference between the two solubility parameters, the poorer the solubility. Based on the method, the micro plastic in the environment medium is measured by calculating the solubility parameter for the first time, pollutants (including the micro plastic and other components) in the sediment are extracted by adopting high temperature and high pressure, the micro plastic is dissolved in the extract, the solubility parameter of the extract is changed by adding other solvents, so that the solubility parameter of the extract is greatly different from the solubility parameter of the micro plastic, the micro plastic is separated out, other co-extracted components are still in the solution, the micro plastic is further filtered, and the micro plastic is detected by adopting mature infrared spectroscopy.
The solubility parameter of a substance is defined as: the square root of the energy of vaporization per unit volume of a substance is a parameter value that characterizes the strength of the simple liquid intermolecular interaction, expressed as δ, and is given by the formula:
δ(ΔEv/V)1/2 (1-1)
wherein, delta is solubility parameter, (J/cm)3)1/2；ΔEvV is the energy of gasification per unit volume of the substance, also called cohesive energy, J/cm3。
By calculating the solubility parameter of the polymer and comparing it with the solubility parameter of the solvent, the degree of solubility between the polymer and the solvent can be quantitatively characterized. According to the calculation model, the closer the solubility parameters of the polymer and the solvent are, the higher the solubility of the polymer is; conversely, the greater the difference in solubility parameters between the polymer and the solvent, the lower the degree of solubility of the polymer, and the more likely it will precipitate in the solvent.
The application establishes a new method for analyzing and detecting the micro-plastic in the sediment based on the calculation of a solubility parameter on the basis of a pressurized fluid extraction method (PFE). The extract obtained by pressure extraction is concentrated, the solvent composition proportion is adjusted according to the calculation result of solubility parameters, a solvent system with larger difference with the solubility of the micro-plastic is selected for selective precipitation of the micro-plastic, and the obtained extract is subjected to gravimetric analysis and infrared spectrum detection, so that qualitative and quantitative analysis of the micro-plastic in the sediment is realized. The established method was further validated by the detection of micro-plastics in the actual sediment samples. The method can provide a new idea for measuring and extracting the micro-plastics in the complex media such as soil, sediment, indoor dust and the like.
Referring to fig. 1-5, the technical solution of the present application will be described in detail with reference to the following embodiments.
1 experimental part
1.1 instruments and reagents
The instrument comprises the following steps: ASE-350 Rapid solvent extraction (ASE) (Thermo, USA),
RV10 basic rotary evaporator, solvent filter (Jinteng) (with 0.22 μm glass fiber filter membrane), Fourier transform infrared spectrometer (Nicolet iS10), XP205 electronic balance (Mettler Toledo, Switzerland).
Reagent: dichloromethane (dichromethane, DCM), Methanol (Methanol, MeOH), Acetonitrile (ACN), isooctane (iso-octane) and n-Hexane (n-Hexane) (HPLC grade, 99.9%, j.t. baker), potassium bromide (KBr, 99.99%, metal analysis,
)。
and (3) standard substance: polypropylene (PP), Polyethylene (PE), polystyrene (poly (styrene), PS), Polycarbonate (PC), Polyvinyl chloride (PVC), Polyethylene terephthalate (PET). The microplastic used in this experiment was purchased from Shanghai Yuanjin industries, Inc., where PE microplastic d50About 20 μm, PET microplastic d50About 50 μm, the remaining 4 types of microplastics d50Are all about 80 μm.
1.2 Experimental methods
Accurately weighing 10.00g of sediment sample, adding the sediment sample into an ASE extraction pool, respectively adding about 10.00mg of 6 standard micro-plastics of PP, PE, PS, PC, PVC and PET, adding diatomite with the same volume as the sample, uniformly mixing, and performing accelerated solvent extraction according to the following conditions: extracting solvent: dichloromethane; the temperature is 180 ℃, the pressure is about 1500psi, the leaching volume is 80%, the heating is carried out for 9min, 3 static cycles are carried out, the purging time is 75s, and the standing time is1 min.
To further verify the influence of the solubility parameters on the selective precipitation of the microplastics, the collected extracts were treated in 3 different ways: (a) directly carrying out suction filtration; (b) concentrating to about 10 mL; (c) after concentrating to 10mL, the solubility parameter of the system is adjusted: (c)1) Adding a solvent with different solubility parameters from the micro plastic (wherein, an acetonitrile solvent is added into PP and PE, and an isooctane solvent is added into PS, PC, PVC and PET) to 100 mL; (c)2) Methanol which has larger difference with the solubility parameter of the micro-plastic is added as a solvent to be 100mL, and the solution is filtered by a solvent filter. The filters were dried, weighed, and subjected to compositional identification using a Fourier transform infrared spectrometer (Nicolet iS10) to obtain a spectrogram. The specific extraction and analysis process is shown in FIG. 1. This experiment was repeated 3 times for a total of 72 experiments.
In order to deduct interference of micro-plastics in sediment background, the application further sets up parallel control group experiments: and (3) uniformly mixing 10.00g of sediment and the diatomite with the same volume, and treating according to the experimental steps to obtain the mass and the spectrogram of the background medium-micro plastic.
The detector type of the Fourier transform infrared spectrometer (Nicolet iS10) iS DTGS/KBr, and the wave number range iS 400--1The sample scanning times are as follows: 32 times, resolution: 4.00cm-1. And comparing the spectrum with a standard product spectrum library (OMNIC spectrum library), and defining the sample corresponding to the spectrum with the matching degree of 70% or more as the micro-plastic so as to determine the components of the micro-plastic.
1.3 solubility parameter calculation
(1) The solubility parameter of the micro plastic is calculated by adopting a group contribution method, and the calculation formula is as follows:
δ＝ρ∑Fi/M (1-2)
where ρ is the density of the polymer, M is the molecular weight of the polymer chain segments, FiIs the molar attraction constant of each group component in the polymer molecule. Pass meterThe delta values of the 6 microplastics of the application were calculated and are shown in Table 1.
TABLE 16 Delta values of the microplastics
(2) The values of the solubility parameters of the individual solvents are referred to in the literature and are shown in Table 2.
TABLE 2 delta values for single solvents (298.15K)
(3) The solubility parameter of the mixed solution was calculated according to the following formula:
in the formula phii，δiIs the volume fraction and solubility parameter of the i-th component solvent, the sum of the volume fractions of all solvents ∑ ΦiIs 1. The delta values of the obtained mixed solvent are calculated and shown in Table 3.
TABLE 3 Delta value of the solvent mixture (298.15K)
2 results and discussion
2.1 Effect of different precipitation methods on the recovery of Microplastic from sediment
To investigate the effect of solubility parameters on the selective precipitation of microplastics, the collected extracts were treated as follows: (a) direct suction filtration, only PP and PE micro-plastics are obviously separated out in experiments, which is caused by DCThe solubility parameters of M are different from those of PP and PE, and the values of-Delta-are 2.86 and 1.42 (J.cm), respectively-3)1/2Resulting in lower solubility of PP and PE in DCM at room temperature and pressure, and solubility parameters of DCM are closer to those of the 4 microplastics PS, PC, PVC and PET,. DELTA.. delta. DELTA.DELTA.L values of 0.29, 0.41, 0.15 and 0.69 (J. cm. sup. sup-3)1/2Therefore, no significant precipitation was observed; (b) the extracting solution is concentrated by adopting a rotary evaporator, and the micro-plastic is precipitated by reducing the solvent, but the micro-plastic is not significantly precipitated when the extracting solution is concentrated to about 10mL in an experiment, and other co-extracts in the extracting solution are gradually precipitated due to the difference of solubility, which indicates that the concentration mode is difficult to realize the selective precipitation of the micro-plastic; (c) in order to realize the selective precipitation of the micro-plastic, different solvents are further adopted to adjust the solubility parameter of the system. Selecting acetonitrile for PP and PE, and adding to make the solubility parameter of the solvent system and the difference value Delta | of PP and PE respectively 6.87 and 5.43(J cm)-3)1/2Isooctane is selected for PS, PC, PVC and PET, and the values of | Δ δ | are 4.71, 4.59, 4.85 and 5.69(J · cm), respectively-3)1/2The recovery rates obtained are shown in table 4. In order to obtain more accurate recovery rate, the recovery rate calculation of the application is calculated after the background of the sediment is deducted through a parallel test. Under 3 different treatment modes, the recovery rate of PP micro plastic is higher than 93%, and calculation shows that the difference between the solubility parameter of PP and DCM is large, so that almost complete precipitation is realized at normal temperature and normal pressure. For PET micro plastic, the recovery rate is lower under 3 treatment modes, and the recovery rate is below 30%. In order to investigate the accuracy of the established method, the application designs two sets of spiking experiments for verification: uniformly mixing a PET micro-plastic standard substance with diatomite (simulated sediment), and performing ASE extraction: in the first group, the extracting solution is dried by slow flow nitrogen, and the result shows that the recovery rate is more than 95 percent; and in the second group, the extracting solution is concentrated and then added with methanol for suction filtration, and the recovery rate is more than 85 percent. It follows that the low recovery of PET microplastic in the sediment may be due to the sediment environment. Studies have shown that humic acid in river sediments contains more carbonyl functional groups, while the chemical structure of PET microplasticTwo carbonyl functional groups exist in the PET adsorbent, and the adsorption of PET in the deposit is enhanced according to the principle of 'similar phase and solubility', so that the recovery rate is low.
TABLE 4 normalized recovery (%) and precision RSD (%, n. about.3) for the different precipitation methods
(a) Directly carrying out suction filtration; (b) concentrating; (c) after concentration, adjusting the solubility parameter of a solvent system: (c)1) Separating out PP and PE micro-plastics by using acetonitrile, and separating out PS, PC, PVC and PET4 micro-plastics by using isooctane; (c)2)6 kinds of micro plastics are separated out by methanol.
As can be seen from FIG. 2, the recovery rate of the micro-plastic after the direct filtration (a) and the concentration (b) is not obviously improved, but the solvent system is adjusted by using the calculation result of the solubility parameter established in the present application (c)1) Then, the recovery rates of other 4 kinds of micro-plastics except PP and PET are obviously improved, which shows that increasing the difference value | delta δ | of the solubility parameter of the solvent system and the micro-plastics plays a role in promoting the selective precipitation of the micro-plastics. Further adjusting the solubility parameter of the solvent system by adding methanol which has a greater difference from the solubility parameter of the microplastic (c)2) The solubility parameter of the solvent system and the difference values Delta delta | between PP, PE, PS, PC, PVC and PET are respectively 11.88, 10.44, 9.31, 9.43, 9.17 and 8.33 (J.cm)-3)1/2The effect on the precipitation of 6 types of microplastics was observed, and the recovery rates obtained are shown in FIG. 2 (c)2) As shown. By (c) in FIG. 21) And (c)2) The results show that the recovery rates of PE, PS, PC and PVC are further improved, the obtained recovery rates are in a stable range, and the correlation between the | delta | value and the precipitation amount of the micro-plastics is verified.
2.2 Effect of different precipitation methods on the identification of the constituents of the Microplastics
In the application, under 3 different treatment modes of 6 kinds of micro-plastics, due to different reagents, selectively separated components can cause different influences on the identification of the micro-plastic components, and the identification results are as followsAs shown in fig. 3. As can be seen from FIG. 3, the values in a, b, c1Under the mode treatment, the infrared spectrogram of 6 kinds of micro-plastics is compared with the spectrum of standard micro-plastics in a fingerprint area (the wave band is 500-1500 cm)-1) There will be a hetero-peak interference at c2Under the mode treatment, the integral peak shape of the spectrogram is consistent with that of a standard micro plastic spectrogram, and the matching degree is higher. The results of matching data with the spectral library are shown in table 5.
As can be seen from FIGS. 3(1) and (2), the results are shown in a, b and c1Under the mode treatment, PP and PE micro plastic are in a fingerprint area (the wave band is 500-1500 cm)-1) The waveform obviously moves upwards, and the interference of a foreign peak exists, which indicates that the existence of organic matters in a solvent and sediments can cause certain influence on the identification of the components of the micro-plastic in the precipitation process of the micro-plastic, and the quality of a spectrogram can be influenced because the organic matters and other impurities in the sediments exist between pores of a micro-plastic sample in the FTIR detection process. But as a whole at c2The spectrogram obtained in the processing mode is higher in matching degree with the standard micro plastic spectrogram.
From fig. 3(3), it can be seen that under the two treatment modes of a and b, the recovery rate of PS micro-plastics is low, and the obtained spectrogram is searched by a spectrogram library, and the matching degree with the PE spectrogram reaches 90.11% and 85.45%, because the PE micro-plastics background exists in the sediment after infrared detection, as shown by the blank contrast in fig. 3, the characteristic peak of the spectrogram is covered by the spectrogram of the PE micro-plastics in the sediment. c. C1In the treatment mode, the PS spectrogram is 1796, 1749, 1714, 1688 and 1641cm-1And a mixed peak appears, and compared with the infrared spectrogram of the standard micro plastic, the mixed peak has certain difference, and matched polymers are not obtained through spectral library retrieval. At c2Under the processing mode, the matching degree of the spectrogram and the standard spectrogram is high. From FIG. 3(4), it can be seen that the recovery rate of PC micro-plastic is low in both the treatment methods a and b, and no matched polymer is obtained by searching the spectrum library. At c1And c2Under the treatment mode, the obtained spectrogram has high matching degree with the standard micro plastic spectrogram. In addition, the particle size of the original PC micro-plastic standard product is larger than that of micro-plastic obtained by ASE extraction and recovery, so that the micro-plastic standard product is arranged in a fingerprint region (the wave band is 500-1460 cm)-1) The peak shape ofAfter extraction, the particle size of the micro plastic is reduced, the surface is smoother, and the distribution is more uniform, so that a spectrogram with better quality is obtained. Research shows that the requirements on surface smoothness, thickness and the like of a sample are high during detection of an infrared spectrometer, the surface of the sample is rough, and scattering easily occurs to weaken spectrogram signals, so that interference is caused on the quality of the spectrogram.
As shown in FIGS. 3 and 5, the PVC micro-plastic is shown in a, b and c1In the treatment mode, the fingerprint area (wave band 500-1500 cm)-1) The peak shape of the PE is obviously different from the infrared spectrogram of the original micro plastic, the peak shape is unclear and is mostly a mixed peak, the characteristic peak of the PE is obtained in a processing mode through searching a spectral library, and the characteristic peaks of the PE are obtained in b and c1Under the treatment mode, the obtained spectrogram has low matching degree with PVC, and the type of the polymer cannot be judged. And at c2Under the processing mode, the matching degree of the infrared spectrogram and the standard spectrogram is higher. From fig. 3(6), it can be seen that, in both the treatment methods a and b, the obtained spectra were searched with the OMNIC library, and no matched polymer was obtained. At c1In the treatment mode, the degree of matching between the obtained spectrogram and PET was 69.06%, and the type of the polymer could not be determined. At c2Under the treatment mode, the obtained spectrogram has higher matching degree with the infrared spectrogram of the original standard micro plastic.
In summary, after the extracting solution obtained by ASE extraction is concentrated, a methanol solvent with a larger difference with the solubility parameter of the micro-plastic is added, so that the micro-plastic can be more completely separated out, no obvious impurity interference exists, the obtained infrared spectrogram has higher matching degree with the standard spectrogram, and the selective separation and detection of the micro-plastic in a complex medium can be realized.
TABLE 5 identification results of 6 microplastics in the sediment by different treatment modes
nd: not detected (not detected).
2.3 Co-precipitation of Mixed Microplastics
In order to more comprehensively explore the precipitation condition of micro-plasticsThe study further carried out a mixed micro-plastic labeling experiment: weighing 10.00g of dried sediment sample, putting the sediment sample into an ASE extraction pool, adding about 2.00mg of 6 kinds of micro-plastics, adding equal volume of diatomite, uniformly mixing, carrying out ASE extraction according to the steps of the 1.2 experimental method part, carrying out rotary evaporation on the obtained extract, and respectively carrying out ASE extraction according to c1And c2The step (2) is processed. The results show that1After treatment, the total recovery rate of the obtained mixed micro-plastic is 77.94 percent2After treatment, the total recovery of the mixed micro-plastic was 81.08%, and the obtained infrared spectrum is shown in FIG. 4.
The peak position of the infrared standard spectrogram characteristic peak of 6 types of micro-plastics can be known from a spectrum library as shown in Table 6. The positions of 3085, 3060, 3026, 2951, 2919, 2850, 1776, 1725, 1601, 1505, 1453, 1376, 1232, 1194, 1164, 1081, 1015, 972, 832, 758, 698cm appear when observing the characteristic peaks of the infrared spectrogram of the mixed standard in the graph in FIG. 4-1The number of peaks at around the constant wave number was coincident with the position of the single-standard characteristic peak, and thus it was possible to determine that the microplastic co-precipitated. Combining the characteristics of the infrared spectroscopy, on the basis of a pretreatment technology based on solubility parameter calculation, the method can preliminarily determine the nature of the micro-plastic components with the standard spectrogram in the sample, and can further adopt the technologies such as Pry-GC-MS and the like to qualitatively identify unknown components.
TABLE 6 characteristic peak position/(cm-1) of infrared standard spectrogram of microplastic
2.4 actual sample application
The method for selectively precipitating the micro-plastic based on the solubility parameter calculation is applied to detect and analyze 30 sediment samples collected from the yellow river delta area, and the sample amount is 30 g. Table 6 summarizes the micro-plastic concentration distribution and type in the collected sediment, and fig. 5 is an infrared spectrum of the micro-plastic in the sediment of yellow river delta. The result shows that 4 kinds of micro-plastics are detected, namely PE, PS, PP and PVC, and the detection rate range is 3.33% -73.33%, wherein the detection rate of PE is the highest, and the detection rates of other 3 kinds of micro-plastics are all lower than 20%. Research has shown that fishery is the main source of micro-plastics in coastal areas, and PE is commonly used for materials such as packaging and fishing gear. Thus, plastic contamination from fisheries and river importation may be the major source of micro-plastics in sediments in the yellow river delta area. Microplastic pollution studies conducted by Zhanjiang mangrove wetland sediments also found that PE accounts for the highest proportion, and that region for fishery farming, river intake, and deposition of microplastic in seawater are the major sources of microplastic, and are in substantial agreement with the results of this application.
TABLE 6 distribution and type of microplastic concentration in yellow river Delta sediment
Table6 concentrations and types of microplastics in sediments of Yellow River Delta
The application establishes a method for detecting micro-plastics in sediments based on solubility parameter calculation. The selective precipitation of the micro-plastic is realized by adjusting the solubility parameter of the solvent system and the difference value delta of the micro-plastic. The result shows that the increase-delta-sigma value can promote the selective precipitation of the micro-plastics, and a new idea is provided for the extraction and analysis of the micro-plastics in complex media such as soil, sediment, indoor dust and the like.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (7)
1. A method for detecting micro-plastics in deposits based on solubility parameter calculation, comprising:
step 1: weighing a proper amount of freeze-dried sediment sample, adding the freeze-dried sediment sample into an ASE extraction pool, adding diatomite with the same volume as the sample, uniformly mixing, and performing accelerated solvent extraction according to the following conditions:
extracting solvent: dichloromethane; the temperature is 180 ℃, the pressure is 1500psi, the leaching volume is 80%, the heating is carried out for 9min, 3 static cycles are carried out, the purging time is 75s, and the standing time is1 min;
step 2: treating the extracted extract by adopting the following method: concentrating the extracting solution, calculating the solubility parameter of the micro-plastic, selecting a solvent with a larger difference value with the solubility parameter of the micro-plastic, adding a proper amount of the solvent into the concentrated extracting solution, after the micro-plastic is fully separated out, performing suction filtration by using a solvent filter, drying and weighing the filter membrane, slightly scraping the extract on the filter membrane, and analyzing and detecting by using a Fourier transform infrared spectrometer.
2. The method for detecting the micro-plastic in the sediment based on the calculation of the solubility parameter as claimed in claim 1, wherein the micro-plastic is one or a mixture of PP, PE, PS, PC, PVC and PET 6.
3. The method for detecting the micro-plastic in the sediment based on the solubility parameter calculation is characterized in that the solubility parameter of the mixture of the micro-plastic can be calculated by a group contribution method according to the following formula:
δ＝ρ·∑Fi/M
wherein, FiIs the molar attraction constant of each group in the molecule, ρ is the density of the polymer, and M is the molar mass of the polymer mer.
4. The method for detecting micro-plastic in sediment based on solubility parameter calculation as claimed in claim 1 or 2, wherein the solvent is a mixed solution, and the solubility parameter of the mixed solution is calculated according to the following formula:
in the formula phii，δiIs the volume fraction and solubility parameter of the i-th component solvent, the sum of the volume fractions of all solvents ∑ ΦiIs 1.
5. The method for detecting the micro-plastic in the sediment based on the calculation of the solubility parameter as claimed in claim 4, wherein the mixed solution is one or a mixture of several of dichloromethane, isooctane, acetonitrile and methanol.
6. The method for detecting the micro-plastic in the sediment based on the calculation of the solubility parameter as claimed in one of claims 1 to 3, wherein in the step 2, the components and the approximate proportion of the micro-plastic are determined according to the environmental survey result of the sample collection place.
7. The method of claim 1-6, wherein the difference between the solubility parameter of the micro-plastic and the solubility parameter of the solvent is designated as |. DELTA. |, |. DELTA. | is not less than 3.
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