CN111220434A - Method for extracting soil metal nanoparticles - Google Patents
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- CN111220434A CN111220434A CN202010054086.1A CN202010054086A CN111220434A CN 111220434 A CN111220434 A CN 111220434A CN 202010054086 A CN202010054086 A CN 202010054086A CN 111220434 A CN111220434 A CN 111220434A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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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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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G01N1/4077—Concentrating samples by other techniques involving separation of suspended solids
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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/42—Low-temperature sample treatment, e.g. cryofixation
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- G—PHYSICS
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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
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Abstract
The invention discloses a method for extracting soil metal nanoparticles, which comprises the following steps: air-drying the soil, grinding and sieving, and uniformly mixing the sieved soil; adding high-purity water into the uniformly mixed soil, horizontally vibrating and dispersing the water-soil mixture, adding the high-purity water after the vibration is finished, and uniformly mixing to obtain a soil solution; carrying out ultrasonic dispersion treatment on the soil liquid, and then removing supernatant after sedimentation and layering to obtain a soil clay component; carrying out ultrasonic dispersion treatment on the soil clay component, carrying out centrifugal treatment on the soil clay component after ultrasonic treatment, and extracting supernatant to obtain a soil metal nanoparticle precursor; filtering the soil metal nanoparticle solution precursor by using the carbon nano film to obtain a soil metal nanoparticle solution; and (3) carrying out freeze drying treatment on the soil metal nanoparticle solution to obtain the soil metal nanoparticles.
Description
Technical Field
The invention relates to the field of soil chemistry, in particular to a method for extracting soil metal nanoparticles.
Background
Soil metal Nanoparticles (Mineral Nanoparticles) refer to crystalline and amorphous solid materials having a particle size of about 1-100 nm formed during natural soil formation. Nanoparticles are very common in soil and are the most important constituent of environmental nanoparticles. Research shows that the nano particles in the soil are important carriers of elements in the environment and have important influence on the biogeochemical process of the elements; it controls the migration, transformation, circulation and biological effectiveness of heavy metal and organic pollutant in soil to reach the effect. It strongly influences important environmental processes such as soil occurrence, soil physicochemical properties and environmental quality evolution. In addition, the synthesized nano particles such as nano ferric oxide and the like are new materials for controlling soil pollution, and have wide application prospects in the aspects of removing heavy metals and persistent organic pollutants in soil and controlling polluted environment. Therefore, understanding the surface structure, micro-morphology, interface behavior and function of nanoparticles in soil environment and their environmental effect mechanism are an important development trend in the soil and environmental field. The method has important theoretical significance for understanding the migration, transformation and self-purification of heavy metal and organic pollutants in the soil effect, and is also an important theoretical basis for developing nano materials to restore polluted environment. For example, Hochella published a related paper in Science, 21Mar 2008: 1631-.
It is worth pointing out that nanotechnology is a new technology that is widely used. Environmental applications of synthetic nanoparticles will cause these substances to enter the environment. It is important to assess the environmental risks of these artificial nanoparticles, such as their mobility, reactivity, ecotoxicology, persistence and health impact. Therefore, extracting nanoparticles from soil is an important technology for understanding and studying the physicochemical characteristics of soil nanoparticles and their environmental behaviors. Because soil nanoparticles have specific characteristics that are different from other macro-particles and micro-molecules, they have many unique physical and chemical characteristics. In order to understand these characteristics, environmental behavior and effects of nanoparticles in soil, it is necessary to separate and extract these nanoparticles from the soil. At present, a method system for soil nano-science research is still explored, and a systematic method for separating and extracting soil nano-particles is lacked.
At present, the main methods for separating and extracting soil metal nanoparticles mainly comprise a vibration-sedimentation method, a chemical dispersion-sedimentation method, a centrifugal method and an ultrafiltration method. The methods mainly solve the extraction problem of the nanoparticles, but the nanoparticles in the soil have various shapes and have obvious interaction with different components in the soil, such as organic matters, the separation effect of different nanoparticles is not ideal, and the chemical dispersion has the defects of environmental risk, insufficient dispersion degree of physical dispersion, long extraction time, small extraction amount, uneconomic performance and the like; in addition, the operation conditions of the currently adopted extraction method are not strict enough, and human errors are easily introduced into the extracted products, particularly the granularity; the extracted nanoparticles have large variation in particle size range, lack uniform standards, and cannot ensure the parallelism and accuracy of analysis. Particularly, an effective method for extracting metal nanoparticles from contaminated soil is lacked at present.
Disclosure of Invention
The invention mainly solves the technical problem of providing an efficient and accurate method for extracting metal nanoparticles in soil, which comprises the following steps: s1, grinding and sieving: removing surface soil from a soil sample to be extracted, taking a proper amount of soil, air-drying, grinding and sieving, and uniformly mixing the sieved soil; s2, preparing soil liquid: adding high-purity water into the uniformly mixed soil, horizontally vibrating and dispersing the water-soil mixture, adding the high-purity water after the vibration is finished, and uniformly mixing to obtain a soil solution; s3, preparing soil clay components: carrying out ultrasonic dispersion treatment on the soil liquid, standing and settling, calculating the settling time of the soil metal nanoparticles with the particle size of less than 100nm settling to a certain specific position according to the temperature of the soil liquid and a Stokes equation, and then removing supernatant after settling and layering to obtain a soil clay component; s4, centrifugal extraction: carrying out ultrasonic dispersion treatment on the soil clay component, carrying out centrifugal treatment on the soil clay component after ultrasonic treatment, and extracting supernatant to obtain a soil metal nanoparticle precursor; s5, filtering by using a carbon nano-film: filtering the soil metal nanoparticle solution precursor by using a carbon nano film to obtain a soil metal nanoparticle solution; and S6, carrying out ultralow-temperature freezing preservation on the soil metal nanoparticle solution, and carrying out freeze drying treatment after the soil metal nanoparticle solution is completely frozen to obtain the soil metal nanoparticles.
The method for extracting the metal nanoparticles in the soil can fully disperse the metal nanoparticles in the soil without adding any chemical reagent, ensures the natural original structure of the nanoparticles in the soil, can reduce the loss of the metal nanoparticles in the soil in the dispersion process and the extraction process to the maximum extent, and can quickly and effectively extract a large amount of metal nanoparticles in the soil.
In a preferred embodiment, a reverse osmosis purification step is added between the step S3 and the step S4: removing impurities from the soil clay component by using a reverse osmosis membrane; the impurities include at least one of dissolved salts, colloids, microorganisms, and organic substances.
In a preferred embodiment, a reverse osmosis purification step is added between the step S4 and the step S5: removing impurities from the soil metal nanoparticle precursor by using a reverse osmosis membrane; the impurities include at least one of dissolved salts, colloids, microorganisms, and organic substances.
In a preferred embodiment, a reverse osmosis purification step is added between the step S5 and the step S6: removing impurities in the soil metal nanoparticle solution by using a reverse osmosis membrane; the impurities include at least one of dissolved salts, colloids, microorganisms, and organic substances.
In a preferred embodiment, the weight ratio of the soil to the used high purity water in step S2 is 1: 1-1: 200.
in a preferred embodiment, the ultrasonic dispersion treatment method in step S3 is to use an ultrasonic cell disruptor.
In a preferred embodiment, an ultrasonic dispersion step is added between step S3 and step S4, and the soil clay component is dispersed using an ultrasonic cell disruptor.
Drawings
The invention and its advantages will be better understood by studying the following detailed description of specific embodiments, given by way of non-limiting example, and illustrated in the accompanying drawings, in which:
fig. 1 is a Transmission Electron Microscopy (TEM) picture observing the particle diameter of the prepared metal nanoparticles.
Fig. 2 is another Transmission Electron Microscopy (TEM) picture observing the particle size of the prepared metal nanoparticles.
Detailed Description
The word "embodiment" is used herein to mean serving as an example, instance, or illustration. In addition, the articles "a" and "an" as used in this specification and the appended claims may generally be construed to mean "one or more" unless specified otherwise or clear from context to be directed to a singular form.
The following disclosure provides many different embodiments or examples for implementing different features of the invention. To simplify the disclosure of the present invention, the components and arrangements of specific examples are described below. Of course, they are merely examples and are not intended to limit the present invention. In addition, the present invention provides examples of various specific processes and materials, but one of ordinary skill in the art may recognize applications of other processes and/or uses of other materials.
Examples
First, a method for extracting soil metal nanoparticles according to an embodiment of the present invention is explained, the method including the steps of:
s1) grinding and sieving: removing surface soil with the thickness of about 10cm from a soil sample to be used, naturally air-drying the residual soil to constant weight, removing broken stone residues, plant roots and branches and other residues in the air-dried soil, coarsely grinding the soil, sieving the soil by a 10-mesh sieve, and uniformly mixing the sieved soil.
S2) preparing soil liquid: adding 100.0g of the uniformly mixed soil and 200.0mL of high-purity water into a 1L glass bottle, horizontally oscillating for 6 hours at the temperature of 20 ℃ at 150rpm, adding 600.0mL of high-purity water after oscillating and resolving the stagnation, and oscillating and shaking uniformly to obtain a soil solution.
S3) soil clay component preparation: performing ultrasonic dispersion treatment on the soil liquid by using an ultrasonic cell disruptor, and performing ultrasonic treatment for 33min and 20s at a rated power of 10% (1200W multiplied by 10% ═ 120W);
and standing the soil liquid subjected to ultrasonic treatment, naturally settling the soil liquid for 35h 44min, calculating the settling time according to the temperature of the soil liquid and a Stokes equation, and transferring the upper-layer suspension into a 1L centrifugal bottle by using a peristaltic pump after the settling is finished to obtain the soil clay component.
S4) subjecting the soil clay component to ultrasonic dispersion treatment by using an ultrasonic cell disruptor, and performing ultrasonic treatment for 4min 10S at a rated power of 10% (1200W × 10% ═ 120W);
centrifuging the ultrasonically treated soil clay component by using a centrifuge (Beckman Coulter, model Avanti JXN-26, rotor JLA-8.1000, based on Stokes' law formula), wherein the centrifuging parameters are as follows: ROTORF 0685; RPM 5200; TIME 11; TEMP ═ 20; ACCE is 0; DEACCE is 0, and the supernatant, i.e., the soil nanoparticle solution, is obtained.
S5) reverse osmosis purification: the soil clay component is purified to remove impurities therein using a reverse osmosis membrane, which uses polyvinyl alcohol (PVA) with a negatively charged surface in order to inhibit the adsorption of contaminants on the membrane by charge repulsion since contaminants (fouling substances) in the treated soil are generally negatively charged, and has a spiral membrane structure. The reverse osmosis purification method comprises the following steps: the control system opens the sample injection valve and the sample outlet valve to carry out reverse osmosis for the first time, the soil clay component enters from the sample injection valve, and the impurity solution enters the central liquid collecting pipe under the action of the filter element reverse osmosis membrane, so that impurities such as dissolved salts, colloids and microorganisms flow out through the outlet of the central liquid collecting pipe. The soil clay component with impurities removed is gathered near the pressure balloon, and flows out through the sample outlet valve after the pressure balloon is compressed. Detect when pressure sensor and get rid of impurity soil clay component pressure rises to given pressure, and control system control closes the sampling valve and goes out the appearance valve and carry out reverse osmosis purification for the second time, and the pressure sacculus receives the pressure counteraction that the compression of soil clay component produced soil clay component, soil clay component is reverse to carry out the reutilization through the filter core for the impurity solution that generates gets into central collecting tube, and the export of back edge central collecting tube flows, and the pressure that the pressure sacculus produced reduces along with the output of impurity solution, and pressure sensor detects soil clay component lateral pressure falls to given pressure, and sampling valve and play appearance valve are opened in control system control, and the reverse osmosis purification of once more repeatedly carries out.
And (3) filtering the carbon nano film after reverse osmosis purification: and filtering the precursor of the soil metal nanoparticle solution by using a carbon nano film, adsorbing nanoparticles of non-metal components by using the carbon nano film, and filtering to obtain the soil metal nanoparticle solution.
S6) transferring the purified soil metal nanoparticle solution into a plastic small bottle, sealing the bottle mouth with tinfoil, pricking a plurality of small holes on the tinfoil, and freezing and storing in a refrigerator at-80 ℃; and after the frozen soil metal nanoparticle solution is completely frozen, freeze-drying by using a freeze dryer to obtain the soil metal nanoparticles.
Claims (7)
1. A method for extracting soil metal nanoparticles, which is characterized by comprising the following steps:
s1, grinding and sieving: removing surface soil from a soil sample to be extracted, taking a proper amount of soil, air-drying, grinding and sieving, and uniformly mixing the sieved soil;
s2, preparing soil liquid: adding high-purity water into the uniformly mixed soil, horizontally vibrating and dispersing the water-soil mixture, adding the high-purity water after the vibration is finished, and uniformly mixing to obtain a soil solution;
s3, preparing soil clay components: carrying out ultrasonic dispersion treatment on the soil liquid, standing and settling, calculating the settling time of the soil metal nanoparticles with the particle size of less than 100nm settling to a certain position according to the temperature of the soil liquid and a Stokes equation, and then removing supernatant after settling and layering to obtain a soil clay component;
s4, centrifugal extraction: carrying out ultrasonic dispersion treatment on the soil clay component, carrying out centrifugal treatment on the soil clay component after ultrasonic treatment, and extracting supernatant to obtain a soil metal nanoparticle precursor;
s5, filtering by using a carbon nano-film: filtering the soil metal nanoparticle solution precursor by using a carbon nano film to obtain a soil metal nanoparticle solution;
and S6, carrying out ultralow-temperature freezing preservation on the soil metal nanoparticle solution, and carrying out freeze drying treatment after the soil metal nanoparticle solution is completely frozen to obtain the soil metal nanoparticles.
2. The method for extracting soil metal nanoparticles as claimed in claim 1, wherein: a reverse osmosis purification step is added between the step S3 and the step S4: removing impurities from the soil clay component by using a reverse osmosis membrane; the impurities include at least one of dissolved salts, colloids, microorganisms, and organic substances.
3. The method for extracting soil metal nanoparticles as claimed in claim 1, wherein: a reverse osmosis purification step is added between the step S4 and the step S5: removing impurities from the soil metal nanoparticle precursor by using a reverse osmosis membrane; the impurities include at least one of dissolved salts, colloids, microorganisms, and organic substances.
4. The method for extracting soil metal nanoparticles as claimed in claim 1, wherein: a reverse osmosis purification step is added between the step S5 and the step S6: removing impurities in the soil metal nanoparticle solution by using a reverse osmosis membrane; the impurities include at least one of dissolved salts, colloids, microorganisms, and organic substances.
5. The method for extracting soil metal nanoparticles as claimed in claim 1, wherein: the weight ratio of the soil to the used high-purity water in step S2 is 1: 1-1: 200.
6. the method for extracting soil metal nanoparticles as claimed in claim 1, wherein: the ultrasonic dispersion treatment method in step S3 is to use an ultrasonic cell disruptor.
7. The method for extracting soil metal nanoparticles as claimed in claim 1, wherein: an ultrasonic dispersion step is added between the step S3 and the step S4, and the soil clay component is dispersed by using an ultrasonic cell disruptor.
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| CN114804212A (en) * | 2022-03-29 | 2022-07-29 | 中山大学 | Preparation method of nano goethite |
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