CN110865135A - Method for measuring capacity of micro plastic for adsorbing soil organic chlorine pesticide - Google Patents
Method for measuring capacity of micro plastic for adsorbing soil organic chlorine pesticide Download PDFInfo
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention belongs to the technical field of organic matter detection, and particularly relates to a method for determining soil organochlorine pesticide adsorption capacity of micro-plastic, which comprises the following steps: uniformly mixing the micro plastic particles with a soil sample, adding an organic chlorine pesticide aqueous solution, and sealing and oscillating; taking out the micro plastic particles, drying and weighing; adding an extracting solution into the micro plastic particles for ultrasonic extraction, and filtering the extracting solution to obtain a clear liquid; and blowing the clear liquid by nitrogen, adding n-hexane for dissolving, and detecting by a gas chromatography/electron capture detector. The determination method solves the problem that the micro plastic adsorbs hydrophobic organic matters in the water solution and needs a conversion medium in the determination under the daily scientific research condition.
Description
Technical Field
The invention belongs to the technical field of organic matter detection, and particularly relates to a method for determining soil organochlorine pesticide adsorption capacity of micro-plastics.
Background
The plastic has the advantages of strong plasticity, low manufacturing cost, water resistance, corrosion resistance, good durability and the like, so that the plastic not only has huge consumption, but also has wide application in various fields, and the application of the plastic product is deep in every corner of society. But it is because plastics are chemically stable, corrosion resistant, etc. that they can exist in the environment for a long time and gradually accumulate.
Although the plastic fragments accumulated in the natural environment can not be completely degraded, the plastic fragments are gradually decomposed into a larger number of plastic particles with smaller volume under the influence of natural weathering, sunlight irradiation and the like when the plastic fragments are exposed in the natural environment. Smaller volume means larger specific surface area, and larger specific surface area means more ability to adsorb contaminants, thereby enriching the contaminants.
In recent years, the problem of micro-plastic pollution in soil is increasingly highlighted, wherein the wide application of the mulching film is one of the main sources of the micro-plastic pollution in the soil in China. According to the data of the national statistical bureau, the total usage amount of plastic films in farmland in 2015 is 2603561t, and the usage amount is very large. And the residual mulching film after planting crops is usually physically broken into smaller fragments to be present on the surface layer or inside the soil under the influence of activities such as soil turning, plowing and the like when new crops are planted. The micro-plastics can adsorb hydrophobic organic matters such as organochlorine pesticides and the like, so that pollutants originally in the soil with low content are adsorbed on the micro-plastic particles in a concentrated manner, and the micro-plastic particles existing in the soil for a long time can even enter crop bodies and are enriched in human bodies through food chains to cause great health hazards due to smaller particle sizes.
At present, most of researches relate to the detection of micro-plastics on substances which are easy to dissolve in water, such as heavy metals, antibiotics and the like, for example, the capability and characteristic analysis of the micro-plastics for enriching metal lead elements, which is published by people such as Gaofeng bud, Lijing xi and the like ([ J ] analysis and test report, 2017 (8)), the article takes the micro-plastics as a carrier, and the enrichment capability of the micro-plastics on lead ions in a solution is investigated. However, the method for measuring hydrophobic organic substances such as organochlorine pesticides adsorbed on the micro-plastic is very rare because the water must be removed from the sample before the micro-plastic is installed and the sample has certain requirements for the solvent medium for measuring the sample during sample injection. In addition, in the traditional organic matter extraction methods such as the Soxhlet extraction method and the solid phase extraction method, the plastic can be melted under the required high-temperature condition, the time consumption is relatively long, the large-batch samples cannot be rapidly processed, and the smooth scientific research activity is not facilitated.
Disclosure of Invention
The invention aims to provide a method for measuring soil organochlorine pesticide adsorption capacity of micro-plastic, and solves the problems that the method for measuring organochlorine pesticide in soil in the prior art is complex in steps, long in time consumption and incapable of rapidly processing large-batch samples.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for measuring the capability of micro-plastic for adsorbing organochlorine pesticides in soil comprises the following steps:
step A, uniformly mixing micro plastic particles with a soil sample, adding an organic chlorine pesticide aqueous solution, and sealing and oscillating;
b, taking out the micro plastic particles, drying and weighing;
c, adding an extracting solution into the micro plastic particles for ultrasonic extraction, and filtering the extracting solution to obtain a clear liquid;
d, blowing the clear liquid with nitrogen, adding n-hexane for dissolving, and detecting with a gas chromatography/electron capture detector;
and E, calculating the adsorption capacity according to the detection result in the step D.
Further, the calculation formula in the step E is that the unit adsorption amount of the organic chlorine pesticide by the micro plastic is c/m, where c is the concentration value of the organic chlorine pesticide measured by the gas chromatography/electron capture detector, and m is the mass of the dried micro plastic particles.
Further, the organochlorine pesticide aqueous solution in the step A is prepared from a high-concentration organochlorine pesticide mother solution and deionized water, wherein the volume ratio of the high-concentration organochlorine pesticide mother solution is less than 0.5%; the proportion of the organochlorine pesticide aqueous solution to the soil is 50-100 mL:1 g.
Further, the high-concentration organochlorine pesticide mother liquor consists of the high-concentration organochlorine pesticide and a mother liquor medium, wherein the mother liquor medium is formaldehyde or acetone.
Further, the step A adopts a completely air-dried soil sample, and the sealing oscillation is more than or equal to 12 hours.
Further, the extracting solution in the step C is a mixed solution of n-hexane and acetone in a volume ratio of 1:1, and the ultrasonic extraction time is 45-90 min.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a method for measuring the capability of a micro plastic to adsorb organochlorine pesticides in soil, which can quickly and efficiently process a large number of samples and solves the problem that the micro plastic in an aqueous solution needs a conversion medium in measurement for adsorbing hydrophobic organic matters under the condition of daily scientific research. In addition, the method of ultrasonic extraction also solves the problem that the properties of materials with lower melting points such as plastics and the like can be changed under high temperature conditions in the common method, has better extraction effect on the soil organochlorine pesticide, greatly improves the working efficiency, and provides better basis for subsequent scientific research activities.
Detailed Description
In order to make the implementation objects, technical solutions and advantages of the embodiments of the present invention more clear and more obvious, the embodiments of the present invention will be further described in detail below. The raw materials and equipment used in the following examples are those conventionally used in the art unless otherwise specified.
The preparation of the organochlorine pesticide aqueous solution used in the following examples is as follows: the high-concentration organochlorine pesticide is mixed with a mother liquor medium to prepare a high-concentration organochlorine pesticide mother liquor, and then the high-concentration organochlorine pesticide mother liquor is mixed with deionized water to obtain an organochlorine pesticide aqueous solution.
The high-concentration organochlorine pesticide is one of eight common organochlorine pesticides (namely α -hexachloro, gamma-hexachloro, β -hexachloro, delta-hexachloro, p.p '-DDE, o.p' -DDT, p.p '-DDD and p.p' -DDT), which are all purchased from China center for purchasing standard substances, the mother liquor medium is a medium which is easy to dissolve in water, such as methanol, acetone and the like, and the reason is that the organochlorine pesticide is mostly hydrophobic organic matter, so that the organochlorine pesticide needs to be uniformly dispersed in water by using the medium which is easy to dissolve in water, the volume ratio of the mother liquor in the organochlorine pesticide aqueous solution is less than 0.5%, and the purpose is to avoid the influence of a co-dissolution effect.
Example 1
Three groups of parallel experiments A1, A2 and A3 are set, 0.05g of micro plastic particles and 0.15g, 0.20g and 0.30g of completely air-dried soil samples are respectively weighed in each group of experiments, after uniform mixing, 15mL of organic chloride pesticide aqueous solution with 0.1ppm is added into each group of mixed samples, namely the water-soil ratio of A1-A3 is respectively 100: 1. 75: 1. and 50: 1. sealing and oscillating the mixed sample for 12 hours; taking out the vibrated micro plastic particles from the solution, drying and weighing, and recording the mass as m; adding a mixture of plastic particles with the volume ratio of 1:1, performing ultrasonic extraction for 45min by using 15mL of mixed solution of normal hexane and acetone, filtering the extracting solution, introducing nitrogen to blow dry, and fixing the volume to 1mL by using the normal hexane to be detected. The organochlorine pesticide concentration of a sample to be detected is detected by adopting a gas chromatography/electronic capture detector (GC-ECD), the detected organochlorine pesticide concentration value is marked as c, and the formula is as follows: the unit adsorption amount of the organic chlorine pesticide by the micro plastic is c/m. In this example, eight kinds of organochlorine pesticides were measured and calculated under the above conditions, and the calculation results are shown in table 1.
TABLE 1 adsorption capacity of plastic granules for organochlorine pesticides at different water-soil ratios
As can be seen from Table 1, in 3 parallel experiments A1, A2 and A3, the adsorption of the microplastic to eight organochlorine pesticides is very obvious, and the detection values of all the substances are very close. The water-soil ratio is 50-100: 1, the method has good effect on measuring the capability of the micro plastic particles for adsorbing the organochlorine pesticide.
Example 2
Four groups of parallel experiments B1, B2, B3 and B4 are set, 0.05g of micro plastic particles with the particle sizes of 120 mu m, 180 mu m, 2000 mu m and 3000 mu m and 0.2g of completely air-dried soil sample are weighed in each group of experiments, after the micro plastic particles are uniformly mixed, 15mL of organic chlorine pesticide aqueous solution with the particle size of 0.1ppm is added, and the mixture is sealed and vibrated for 16 hours; taking out the vibrated micro plastic particles from the solution, drying and weighing, and recording the mass as m; adding a mixture of plastic particles with the volume ratio of 1:1, performing ultrasonic extraction for 90min, filtering the extracting solution, introducing nitrogen to blow dry, and fixing the volume to 1mL by using the n-hexane to be detected. The organochlorine pesticide concentration of a sample to be detected is detected by adopting a gas chromatography/electronic capture detector (GC-ECD), the concentration value of the organochlorine pesticide is measured and is marked as c, and the formula is as follows: the unit adsorption amount of the organic chlorine pesticide by the micro plastic is c/m. In this example, eight kinds of organochlorine pesticides were measured and calculated under the above conditions, and the calculation results are shown in table 2.
TABLE 2 adsorption Capacity of different particle size microplastic particles on organochlorine pesticides
As can be seen from Table 2, in the 4-group parallel tests B1, B2, B3 and B4, the four types of microplastics with the particle sizes of 120 μm, 180 μm, 2000 μm and 3000 μm have different degrees of adsorption of organic chlorine. The two experiments B1 and B2 with smaller plastic particle size have more obvious adsorption effect compared with the two experiments B3 and B4 with larger plastic particle size, which is determined by the properties of the plastics with different particle sizes.
Example 3
Three groups of parallel experiments C1, C2 and C3 are set, 0.05g of micro plastic particles and 0.2g of completely air-dried soil samples are weighed in each group of experiments, after the micro plastic particles and the completely air-dried soil samples are uniformly mixed, 15mL of organochlorine pesticide aqueous solution with the concentration of 0.05ppm, 0.10ppm and 0.20ppm are added, and the mixture is sealed and vibrated for 14 hours; taking out the vibrated micro plastic particles from the solution, drying and weighing, and recording the mass as m; adding a mixture of plastic particles with the volume ratio of 1:1, performing ultrasonic extraction for about 45min, filtering an extracting solution, introducing nitrogen to blow dry, and fixing the volume to 1mL by using the n-hexane to be detected. The organochlorine pesticide concentration of a sample to be detected is detected by adopting a gas chromatography/electronic capture detector (GC-ECD), the concentration value of the organochlorine pesticide is measured and is marked as c, and the formula is as follows: the unit adsorption amount of the organic chlorine pesticide by the micro plastic is c/m. In this example, eight kinds of organochlorine pesticides were measured and calculated under the above conditions, and the calculation results are shown in table 3.
TABLE 3 adsorption Capacity of the Microplastics on organochlorine pesticides of different concentrations
As can be seen from the table, the concentration of the organic chlorine pesticide in the aqueous solution of the organic chlorine pesticide in the 3-group parallel tests C1, C2 and C3 has a great influence on the ability of the micro plastic to adsorb the organic chlorine pesticide, the larger the concentration of the organic chlorine pesticide in the aqueous solution, the more the micro plastic particles adsorb the organic chlorine pesticide component, and the adsorption amount of the micro plastic to the organic chlorine pesticide is basically increased in proportion to the times of the increase of the concentration.
Example 4
Three groups of parallel experiments D1, D2 and D3 are set, 0.05g, 0.08g, 0.10g of micro plastic particles and 0.2g of completely air-dried soil samples are respectively weighed in each group of experiments, after uniform mixing, 15mL of 0.1ppm of organochlorine pesticide aqueous solution is added into each group of mixed samples, and sealing oscillation is carried out for 12 hours; taking out the vibrated micro plastic particles from the solution, drying and weighing, and recording the mass as m; adding a mixture of plastic particles with the volume ratio of 1:1, performing ultrasonic extraction for about 80min, filtering the extracting solution, introducing nitrogen to blow dry, and fixing the volume to 1mL by using the n-hexane to be detected. The organochlorine pesticide concentration of a sample to be detected is detected by adopting a gas chromatography/electronic capture detector (GC-ECD), the concentration value of the organochlorine pesticide is measured and is marked as c, and the formula is as follows: the unit adsorption amount of the organic chlorine pesticide by the micro plastic is c/m. In this example, eight kinds of organochlorine pesticides were measured and calculated under the above conditions, and the calculation results are shown in Table 4.
TABLE 4 adsorption capacity of different masses of microplastics on organochlorine pesticides in soil
As can be seen from Table 4, in the 3-group parallel tests D1, D2 and D3, the mass of the micro plastic particles also has a certain influence on the adsorption of the organochlorine pesticide, and the quantity of the organochlorine pesticide adsorbed on the micro plastic decreases with the increase of the mass of the plastic.
Example 5
Setting three groups of parallel experiments E1, E2 and E3, weighing 0.05g of micro plastic particles and 0.2g of completely air-dried soil samples in each group of experiments, uniformly mixing, adding 15mL of 0.1ppm of organic chlorine pesticide aqueous solution, sealing, vibrating for 12h, 16h and 20h respectively, taking out the vibrated micro plastic particles from the solution, drying and weighing, and recording the mass as m; adding a mixture of plastic particles with the volume ratio of 1:1, performing ultrasonic extraction for about 50min, filtering the extracting solution, introducing nitrogen to blow dry, and fixing the volume to 1mL by using the n-hexane to be detected. The organochlorine pesticide concentration of a sample to be detected is detected by adopting a gas chromatography/electronic capture detector (GC-ECD), the concentration value of the organochlorine pesticide is measured and is marked as c, and the formula is as follows: the unit adsorption amount of the organic chlorine pesticide by the micro plastic is c/m. In this example, eight kinds of organochlorine pesticides were measured and calculated under the above conditions, and the calculation results are shown in Table 5.
TABLE 5 adsorption Capacity to organochlorine pesticides at different concussion times
From the above table, the data in the three parallel experiments E1, E2, and E3 are relatively close, which indicates that the adsorption of the organic chloride pesticide by the micro plastic particles has been balanced at 12h, and the experimental data obtained after 12h of oscillation can well represent the adsorption capacity of the organic chloride pesticide by the micro plastic. Therefore, when the capability of the micro plastic for adsorbing the organochlorine pesticide is measured, more than 12 hours should be selected as the oscillation time.
According to the specific embodiments, the method for determining the capability of adsorbing the soil organic chlorine pesticide by utilizing the micro-plastic is established, the sample treatment method is simple, and the detection method is easy to operate. In addition, the invention also obtains the conclusion that the water-soil ratio, the particle size of plastic particles, the concentration of organic chlorine water solution, the quality of plastic and the oscillation time all have certain influence on the measurement result in the measurement process of the capability of the micro plastic for adsorbing the organic chlorine pesticide in the soil.
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 (6)
1. The method for measuring the capability of the micro plastic for adsorbing the soil organic chlorine pesticide is characterized by comprising the following steps of:
step A, uniformly mixing micro plastic particles with a soil sample, adding an organic chlorine pesticide aqueous solution, and sealing and oscillating;
b, taking out the micro plastic particles, drying and weighing;
c, adding an extracting solution into the micro plastic particles for ultrasonic extraction, and filtering the extracting solution to obtain a clear liquid;
d, blowing the clear liquid with nitrogen, adding n-hexane for dissolving, and detecting with a gas chromatography/electron capture detector;
and E, calculating the adsorption capacity according to the detection result in the step D.
2. The method for determining the soil organochlorine pesticide adsorption capacity of the micro-plastic according to claim 1, wherein the calculation formula in the step E is that the unit adsorption amount of the organochlorine pesticide by the micro-plastic = c/m, wherein c is the concentration value of the organochlorine pesticide measured by a gas chromatography/electron capture detector, and m is the mass of the dried micro-plastic particles.
3. The method for determining soil organochlorine pesticide adsorption capacity of the micro-plastic according to claim 1, wherein the organochlorine pesticide aqueous solution in the step A is prepared from a high-concentration organochlorine pesticide mother solution and deionized water, wherein the high-concentration organochlorine pesticide mother solution accounts for less than 0.5% by volume; the proportion of the organochlorine pesticide aqueous solution to the soil is 50-100 mL:1 g.
4. The method for determining the capability of the micro-plastic to adsorb the soil organic chlorine pesticide as claimed in claim 3, wherein the high-concentration organic chlorine pesticide mother liquor is composed of the high-concentration organic chlorine pesticide and a mother liquor medium, and the mother liquor medium is formaldehyde or acetone.
5. The method for determining soil organochlorine pesticide adsorption capacity of the micro-plastic according to claim 1, wherein a completely air-dried soil sample is adopted in the step A, and the sealing oscillation is carried out for more than or equal to 12 hours.
6. The method for determining soil organochlorine pesticide adsorption capacity of the micro plastic according to claim 1, wherein the extracting solution in the step C is a mixed solution of n-hexane and acetone in a volume ratio of 1:1, and the ultrasonic extraction time is 45-90 min.
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