CN109916938B - Method for measuring spatial distribution of organic pollutants adsorbed by soil organic matters - Google Patents

Method for measuring spatial distribution of organic pollutants adsorbed by soil organic matters Download PDF

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CN109916938B
CN109916938B CN201910173951.1A CN201910173951A CN109916938B CN 109916938 B CN109916938 B CN 109916938B CN 201910173951 A CN201910173951 A CN 201910173951A CN 109916938 B CN109916938 B CN 109916938B
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刘兴华
骆永明
章海波
谢寅雨
朱荣生
王怀中
呼红梅
黄保华
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Institute Animal Science and Veterinary Medicine of Shandong AAS
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Abstract

Hair brushThe invention discloses a method for measuring the spatial distribution of organic pollutants adsorbed by soil organic matters. The method adopts13Adsorbing organic pollutants such as C-marked antibiotics on the soil organic matters, and then analyzing the spatial distribution characteristics of the organic pollutants adsorbed by the soil organic matters by using a NanoSIMS technology. The method not only can effectively overcome the difficulty of distinguishing the carbon distribution in the soil organic matters and pollutants, but also can realize the visual display of the two-dimensional spatial distribution characteristics of the organic matters, and can also measure the three-dimensional spatial distribution.

Description

Method for measuring spatial distribution of organic pollutants adsorbed by soil organic matters
Technical Field
The invention relates to a method for measuring the spatial distribution of organic pollutants on soil organic matters after the soil organic matters adsorb the organic pollutants.
Background
The soil is a carrier for the material and energy exchange of an agricultural ecosystem, and is a material basis for the growth of crops and a basis for land life. The soil is used as an important component of the environment, can not only bear pollution from other environment media, but also is a pollution source of other environment media. Once contaminated, the soil will seriously threaten human health and environmental safety. Therefore, the research on soil pollution and mechanism is attracting more and more attention of researchers. Organic pollutants are one of the main pollutants commonly existing in the current environment, and mainly comprise antibiotics, organic pesticides, phenols, synthetic detergents, harmful microorganisms brought by municipal sewage, sludge and fertilization, and the like. Although many classes of organic chemicals have been banned for many years, the residue and contamination of these contaminants remains serious because they are chemically stable, difficult to degrade, or the secondary products of degradation remain toxic to the environment. Soil organic matter is an important component of soil and has an important effect on the adsorption of organic pollutants. Soil organic matters can be divided into active organic matters, inert organic matters and stable organic matters according to the stability difference of the soil organic matters, organic pollutants adsorbed by the soil organic matters with different stabilities have different toxic effects on the environment, for example, the organic pollutants adsorbed by the granular organic matters with higher activity and lower stability can be released again to form secondary pollution along with the increase of the humification degree, and the like. Soil organic matters have complex spatial structures, and the structures have different adsorption and fixation mechanisms for soil organic pollutants and different actions for resisting activities of animals and plants in soil environments, for example, pollutants entering closed organic matter pores are difficult to release. Therefore, the spatial structure characteristics of the organic pollutants adsorbed by the soil organic matters are determined, and a data basis and a scientific basis can be provided for the pollution effect and the environmental risk assessment of the soil organic pollutants.
Currently, researchers combine synchrotron radiation spectroscopy to study the two-dimensional spatial distribution of pollutants in soil by using an energy stack method. The method has strict requirements on experimental condition control, and ideal organic carbon distribution data is difficult to obtain. And the research of the method for distributing organic pollutants on organic matters (the pollutants and the organic matters simultaneously contain carbon) is proved to be incomprehensible.
Disclosure of Invention
In order to solve the dilemma of the current research, the invention provides a novel method for measuring the spatial distribution of organic pollutants adsorbed by soil organic matters. The method adopts13Adsorbing organic pollutants such as C-marked antibiotics on the soil organic matters, and then analyzing the spatial distribution characteristics of the organic pollutants adsorbed by the soil organic matters by using a NanoSIMS technology. The method not only can effectively overcome the difficulty of distinguishing the carbon distribution in the soil organic matters and pollutants, but also can realize the visual display of the two-dimensional spatial distribution characteristics of the organic matters, and can also measure the three-dimensional spatial distribution.
The technical scheme of the invention is as follows: a method for measuring the spatial distribution of organic pollutants adsorbed by soil organic matters is characterized in that,
1) by using13C marking organic pollutants and adsorbing the organic pollutants by soil organic matters13C-marked organic pollutants are vibrated and adsorbed to reach an equilibrium state to obtain adsorption13Soil organic matter of the organic pollutants marked C;
2) is prepared without adding13C, marking soil organic matters of the organic pollutants as a blank control;
3) freezing and forming the soil organic matters obtained in the step 1) and the step 2);
4) slicing the soil organic matters frozen and formed in the step 3), and then carrying out TEM observation;
5) selecting the distribution position of the target organic matter according to the TEM observation result, and recording the coordinate point of the target organic matter;
6) scanning the target organic matter in the step 5) by using a nano ion probe (nano SIMS), positioning a scanning area according to a coordinate point of the target organic matter, and respectively obtaining a nano SIMS picture and an adsorption mark of the soil organic matter13C soil organic matter picture of organic pollutant, adsorption mark13The soil organic matter picture of the C organic pollutants is obviously compared with the unadsorbed soil organic matter picture13C, enriching to obtain a distribution map of the organic pollutants on the upper surface of the soil organic matter particles;
7) and (3) repeatedly scanning the target organic matter in the step 5) by using a nano ion probe (NanoSIMS), wherein the thickness of the eroded organic matter on the surface of the organic matter sample wafer is 15 +/-5 nm after each scanning, and the scanning is repeated for at least 8 times to prepare a three-dimensional space distribution map of the organic pollutants within the thickness of 100 plus one film and 500nm, wherein the thickness can be automatically adjusted according to the experimental requirements.
The organic pollutants are substances which are easily adsorbed by soil organic matters, such as antibiotics (such as ciprofloxacin and the like), organic pesticides, phenols, synthetic detergents and the like, and can also be harmful microorganisms brought by municipal sewage, sludge and fertilization and the like, and also comprise persistent organic pollutants.
Preferably, the step 1) uses soil organic matter adsorption13The specific method of C-labeled organic contaminants is as follows: preparing NaCl solution as background solution for adsorption experiment and preparing NaCl solution with the background solution13C-labeled organic pollutant adsorption solution; then absorbing the organic matter in the absorption liquid by soil13And C, oscillating and adsorbing the organic pollutants marked by C to reach an equilibrium state.
Preferably, the step 2) is: repeating the process of the step 1) and adding no adsorption liquid in the step 1)13C label background solution of organic contaminants.
Wherein, in the adsorption process of the step 1), a certain amount of adsorption can be taken out at different time intervals13C, freezing and storing soil organic matters of the marked organic pollutants, and dynamically monitoring the adsorption process of the ciprofloxacin on the soil granular organic matters.
Preferably, the freeze forming of step 3) is: freezing the soil organic matter into wedge shape at-20 deg.C, preferably fixing the shape of the soil organic matter in aluminum foil paper before freezing, placing at-20 deg.C, freezing to form, and peeling off the aluminum foil paper.
Preferably, the slicing in step 4) is: and (3) cutting the frozen soil organic matter into slices with the thickness of 500nm by using a come ultra-thin freezing slicer in a liquid nitrogen environment.
Preferably, in the step 4), in order to prevent the damage of the slice structure, each slice is dipped by a mascara brush and is spread on a hydrophilic silicon wafer to prevent the organic matter from being curled, and the silicon wafer is taken as a carrying wafer and is then observed by a TEM.
Preferably, the thickness of the corroded organic matter sample surface in the step 7) is 15nm, and the step is repeated for 10 times to prepare a three-dimensional space distribution map of the organic pollutants within the thickness of 150 nm.
The Nano-scale secondary mass spectrometry (SIMS) technology uses the latest SIMS instrument, is developed on the basis of SIMS (Ion mass spectrometry) and TOF-SIMS (time of flight mass spectrometry), and can be used as a technical means for simulating the visualization of the activity of microorganisms in soil and in-situ soil solution. The method can simultaneously analyze 7 ion types, has higher sensitivity and resolution up to 50nm, and therefore, can accurately position the spatial distribution of the carbon-nitrogen stable isotope. The technology of marking the pollutants by the isotopes also effectively overcomes the difficulty of distinguishing organic matters from carbon distribution in the pollutants.
The isotope fractionation characteristic can be used for tracing soil microorganism activities and feedback processes such as organic matter migration and conversion, and is mostly applied to researches such as soil organic matter humification process and aggregate formation mechanism at present. At present, the pollutant distribution is researched by using isotope tracing, radioactive isotopes are mostly adopted, the requirements of the radioactive isotopes on experimental conditions are strict, and the radioactive isotopes can be completed by specially trained laboratory personnel by equipping a special radioactive laboratory, so that the method is not suitable for tracing research required in common experiments. Therefore, the invention adopts the stable isotope to mark the organic pollutant, and then uses the marked pollutant to carry out the adsorption experiment in the soil organic matter, thereby effectively solving the difficulty in the research of the distribution characteristics of the organic pollutant in the organic matter.
At present, embedding agents such as paraffin, resin and the like are mostly used for slicing at home and abroad, and can be cut into slices after being fixed and formed by the embedding agents, but the embedding agents contain organic matters (carbon) which can not be distinguished from the organic matters of soil and the carbon in organic pollutants, so that the embedding agents are not suitable for use. In order to research organic matter slices, foreign researchers propose that sulfur and indium foil are used as embedding agents, high-temperature heating is needed until sulfur powder is molten, then organic matters are put into high-temperature molten sulfur, and partial soil organic pollutants are easily degraded at high temperature (for example, antibiotics can be degraded when the temperature exceeds 40 ℃). In addition, when the indium foil fixes the organic matters, the organic matters need to be pressed into the indium foil, the original natural spatial structure of the organic matters can be damaged in the pressing process, and in conclusion, the existing method for manufacturing the slices at home and abroad is not suitable for the method.
In view of this, the present inventors made the following improvements:
1. the invention provides a method for forming organic matters by using water as an embedding agent and freezing, which does not destroy the space structure of the organic matters and introduce the interference of other organic matters.
2. Slices made by the conventional embedding medium can be subjected to on-machine analysis after being fished out by a copper net in water, the organic matter slices are melted when meeting water, and adsorbed organic pollutants can be diluted and desorbed to influence the subsequent measurement result. Therefore, the inventor designs the mascara brush (namely the mascara brush made of one eyelash) to transfer the organic matter slices of the soil, and the slice transfer by the mascara brush is free from the influence of water and cannot damage the slice.
3. The thickness of the slice is only 500nm, the slice is easy to dry at room temperature, so that the organic slice is curled, and the flat slice cannot be transferred to the silicon wafer, therefore, the whole slice and the transfer process are adopted in a liquid nitrogen environment (the organic slice is ensured to be formed at low temperature), the hydrophilic treatment is carried out on the silicon wafer (because the organic slice is arranged on the conventional silicon wafer, a sample needs to be dried before the NanoSIMS experiment analysis, a sample chamber in the experiment process is in a vacuum state, the organic slice is easy to fall off from the silicon wafer when vacuumized after being dried, the organic slice is coated by ice after the hydrophilic treatment is carried out on the silicon wafer, the organic matter can be well attached to the silicon wafer in the process of ice dissolution at room temperature, and the organic slice cannot fall off even if vacuumized.
The invention has the beneficial effects that: the method not only can effectively overcome the difficulty of distinguishing the carbon distribution in the soil organic matters and pollutants, but also can realize the visual display of the two-dimensional spatial distribution characteristics of the organic matters, and can also measure the three-dimensional spatial distribution, thereby providing a direct and rapid method for researching the spatial distribution characteristics of the organic pollutants adsorbed by the soil organic matters and laying a method foundation for researching the harm of the organic pollutants in the environment in the soil.
Drawings
FIG. 1 is a section distribution diagram of soil granular organic matter under an optical electron microscope, wherein black and dark brown granules in the section distribution diagram are soil granular organic matter;
FIG. 2 shows unadsorbed granular organic matter of soil scanned by a nanometer ion probe13NanoSIMS plot of C;
FIG. 3 shows an adsorption mark13C ciprofloxacin soil granular organic matter, scanning by using nano ion probe technology13Nanosil of CMS picture, dark area in the picture13Marking an enrichment area with the most orange-red enrichment;
FIG. 4 shows an adsorption mark13C ciprofloxacin soil granular organic matter, scanning by using nano ion probe technology13And C, three-dimensional space distribution diagram.
FIG. 5 is a schematic view of a wedge-shaped ark made of aluminum foil paper, i.e. one end of the rectangle is a 45 degree inclined plane.
Detailed Description
Example 1:
1) accurately preparing 0.01mol/L NaCl solution as background solution for adsorption experiment, and preparing the background solution with a certain volume13And C, marking the adsorption solution with the concentration of the ciprofloxacin being 40 mg/kg. Accurately weighing 0.100g of soil granular organic matter in a polytetrafluoroethylene centrifugal tube, wherein the solid-liquid ratio is 1: 10, adsorbing by using granular organic matters (with higher activity) in soil13C, oscillating the ciprofloxacin marked by C for 24 hours at 25 ℃, so that the adsorption can reach an equilibrium state, setting 12 times of different sampling time within 24 hours, dynamically monitoring the adsorption process of the ciprofloxacin on the granular organic matter of the soil, and freezing and storing the sampled granular organic matter sample of the soil when the adsorption time is set to be 2min, 5min, 10min, 15min, 20min, 30min, 1h, 2h, 4h, 6h, 10h and 24 h;
13c-labeled ciprofloxacin was purchased from Cambridge Isotope Laboratories (Cambridge Isotope Laboratories, Inc); marker parameters for ciprofloxacin: min.99% atom%13C；
2) Making a blank control of granular organic matters of soil, namely repeating the process of the step 1) and adding no adsorbent in the step 1)13C-labeled background solution of ciprofloxacin;
3) respectively putting the soil granular organic matter samples taken out in the step 1) and the step 2) into a wedge-shaped ark (shown in figure 5) made of aluminum foil paper, fixing the shape, putting the ark at-20 ℃, freezing and forming, then peeling off the aluminum foil paper, wherein other embedding agents are not required to be added in the process, water is used as the embedding agent, the sample is frozen into ice at low temperature, and the slicing and manufacturing process is operated in a low-temperature environment;
4) making a wedge-shaped soil granular organic matter slice in the step 3), cutting the soil organic matter into a slice with the thickness of 500nm by using a Leica ultrathin freezing slicer in a liquid nitrogen environment, wherein the wedge-shaped soil granular organic matter slice is very small and soft in texture, and in order to prevent the damage of a slice structure, each slice needs to be dipped by using a lash brush pen to transfer the slice to a square (or round with the diameter of 10 mm) hydrophilic silicon slice with the diagonal length of 10mm for tiling so as to avoid the organic matter from being curled, the silicon slice is a carrying slice, the process is carried out under a microscope, organic matter sample particles are prevented from being clustered or overlapped in the slicing making process, and then a TEM observation is carried out, and the result is shown in figure 1;
5) selecting the position of the distribution of the target organic matter according to the TEM observation result, and recording the coordinate point of the target object;
6) transferring the sample to a sample inlet chamber of a nano ion probe instrument, vacuumizing the sample chamber, drying the sample, scanning the target organic matter in the step 5) by using a nano ion probe (nano SIMS) analyzer, positioning the scanning area according to the coordinate point, and respectively obtaining a nano SIMS picture (figure 2) and an adsorption mark of the soil organic matter13C ciprofloxacin soil organic matter picture (figure 3), adsorption mark13Compared with the unadsorbed soil granular organic matter, the soil granular organic matter picture of the ciprofloxacin C has obvious effect13C enrichment (darkened color, enrichment)13The more C, the more orange red), the distribution diagram of the ciprofloxacin on the upper surface of the soil granular organic matter particles is obtained;
the nano ion probe analysis experiment is completed in the nano ion probe laboratory of the institute of geology and geophysics of the Chinese academy of sciences. The initial ion source of the experiment is Cs+The excitation energy of ions is 6kev, the initial electron beam is 1.2-3.8 pA, the secondary ion extraction pressure is 8kev, the transverse resolution is 100-200 nm, the erosion thickness is 15nm, and the coverage range of a scanned sample is 20 multiplied by 20 mu m2. The initial ion beam current remained constant during the experiment.
The electron gun of NanoSIMS can continuously generate the beam compensation current. All detection results are given in image mode, the retention time of the ion image is 15 ms/pixel, the secondary ion image is 256 × 256 pixels.
7) And (3) repeatedly scanning the target organic matter in the step 5) by using a nano ion probe (NanoSIMS), wherein the thickness of the eroded organic matter on the surface of the organic matter sample is 15nm every time of scanning, and repeating for 10 times to obtain a three-dimensional space distribution map (as shown in fig. 4) of the organic pollutants within the thickness of 150 nm.
Example 2:
and 7) repeatedly scanning the target organic matter in the step 5) by using a nano ion probe (nano SIMS), wherein the thickness of the corroded surface of the organic matter sample wafer is 15nm after each scanning, and the three-dimensional space distribution map of the organic pollutants within the thickness of 300nm can be obtained after repeating for 20 times.

Claims (5)

1. A method for measuring the spatial distribution of organic pollutants adsorbed by soil organic matters is characterized by comprising the following steps:
1) by using13C marking organic pollutants and adsorbing the organic pollutants by soil organic matters13C-marked organic pollutants are vibrated and adsorbed to reach an equilibrium state to obtain adsorption13Soil organic matter of the organic pollutants marked C;
2) is prepared without adding13C, marking soil organic matters of the organic pollutants as a blank control;
3) using water as an embedding agent for the soil organic matters in the step 1) and the step 2), and freezing and forming at low temperature;
the low-temperature freezing forming is as follows: before freezing, fixing the shape of soil organic matters in aluminum foil paper, putting the soil organic matters into the aluminum foil paper, freezing the soil organic matters into a 45-degree wedge shape, and peeling off the aluminum foil paper;
4) slicing the soil organic matters frozen and formed in the step 3), and then carrying out TEM observation;
the slice making is as follows: cutting the frozen soil organic matter into slices with the thickness of 500nm in a liquid nitrogen environment; dipping the slices with a brush pen for each slice, and transferring the slices to a hydrophilic silicon wafer for tiling;
5) selecting the distribution position of the target organic matter according to the TEM observation result, and recording the coordinate point of the target organic matter;
6) scanning the target organic matter in the step 5) by using a nano ion probe, positioning a scanning area according to a coordinate point of the target organic matter, and respectively obtaining a nano SIMS picture and an adsorption mark of the soil organic matter13C soil organic matter picture of organic pollutant, adsorption mark13The soil organic matter picture of the C organic pollutants is obviously compared with the unadsorbed soil organic matter picture13C, enriching to obtain a distribution map of the organic pollutants on the upper surface of the soil organic matter particles;
7) and (3) repeatedly scanning the target organic matter in the step 5) by using a nano ion probe NanoSIMS, wherein the thickness of the corroded surface of the organic matter sample wafer is 15 +/-5 nm every time of scanning, and repeating for at least 8 times to prepare the three-dimensional space distribution map of the organic pollutants within the thickness of 100-500 nm.
2. The method for measuring the spatial distribution of organic pollutants adsorbed by soil organic matters according to claim 1, wherein the eroded thickness of the surface of the organic matter sample is 15nm, and the method is repeated for 10 times to prepare the three-dimensional spatial distribution map of the organic pollutants within 150nm of the surface of the organic matter sample.
3. The method for determining the spatial distribution of organic pollutants adsorbed by organic matters in soil according to claim 1 or 2, wherein the organic pollutants are any one of antibiotics, organic pesticides, phenols, synthetic detergents and harmful microorganisms brought by municipal sewage, sludge and fertilizer application.
4. The method for determining the spatial distribution of the soil organic matter adsorbing organic pollutants as claimed in claim 1 or 2, wherein the step 1) uses the soil organic matter adsorption13The specific method of C-labeled organic contaminants is as follows: preparing NaCl solution as background solution for adsorption experiment and preparing NaCl solution with the background solution13C-labeled organic pollutant adsorption solution; then absorbing the organic matter in the absorption liquid by soil13And C, oscillating and adsorbing the organic pollutants marked by C to reach an equilibrium state.
5. The method for determining the spatial distribution of the organic pollutants adsorbed by the organic matters in the soil according to claim 4, wherein the step 2) is as follows: repeating the process of the step 1) and adding no adsorption liquid in the step 1)13C label background solution of organic contaminants.
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