CN114660264B - Soil heavy metal long-term restoration detection method - Google Patents
Soil heavy metal long-term restoration detection method Download PDFInfo
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- CN114660264B CN114660264B CN202210246426.XA CN202210246426A CN114660264B CN 114660264 B CN114660264 B CN 114660264B CN 202210246426 A CN202210246426 A CN 202210246426A CN 114660264 B CN114660264 B CN 114660264B
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
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- G01N1/00—Sampling; Preparing specimens for investigation
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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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- 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
- G01N1/44—Sample treatment involving radiation, e.g. heat
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Abstract
The invention relates to a method for long-term restoration and detection of soil heavy metals. The method comprises the following steps: uniformly mixing the repairing agent with soil to be detected to prepare a soil sample; placing the soil sample in an experimental environment; and carbonizing the soil sample, periodically treating, and sequentially carrying out precipitation treatment, freeze thawing treatment and ultraviolet irradiation treatment on the soil sample in one treatment period. The simulation method for the long-term restoration of the soil heavy metal can effectively predict the failure rule of the effect of stabilizing anions and cations by the restoration agent in the natural environment, reduce the workload and improve the working efficiency.
Description
Technical Field
The invention relates to the technical field of environmental quality evaluation, in particular to a soil heavy metal long-term restoration detection method.
Background
Soil is an important natural resource for human society to survive, and is also the most basic structural unit of the ecological system. With the development of social economy and the improvement of industrial and agricultural productivity, the heavy metal pollution of soil is gradually serious. Heavy metal pollution is different from pollution of other organic compounds, most of the organic compounds can reduce the harmfulness through the self-purification capability in nature, and the heavy metals have mobility and nondegradability, can stay in soil for a long time and gradually accumulate along with ecological cycle. Meanwhile, heavy metal pollution of soil can reduce crop quality and yield, and endanger human health through food chains.
The stabilization is used as a main restoration technology for soil heavy metal pollution, and has the advantages of high restoration effect, low economic cost, wide application range and the like. The method mainly comprises the steps of adding a repairing agent into soil to enable a chemical reaction to change the form of heavy metal, so as to form a heavy metal compound which is lower in mobility, higher in stability and not easy to be absorbed by organisms, thereby reducing the harm of the heavy metal. Therefore, the efficient repairing agent is an important factor influencing the repairing effect of the heavy metals in the soil, and the research and development of the repairing agent are urgent.
However, in the research and development process of the soil restoration agent, long-term waiting and uninterrupted sampling on the soil restoration site are required in order to obtain the soil heavy metal restoration effect, so that the operation difficulty is high, the working period is long, the working efficiency is low, and the research progress of the soil restoration agent and the evaluation efficiency of the soil restoration effect are seriously affected.
Disclosure of Invention
Based on the problems, the problem of low efficiency of evaluating the restoration effect of the soil restoration agent is needed to be solved, and a soil heavy metal long-term restoration detection method is provided.
A soil heavy metal long-term restoration detection method comprises the following steps:
s1: uniformly mixing the repairing agent with soil to be detected to prepare a soil sample;
S2: placing the soil sample in an experimental environment;
s3: and carbonizing the soil sample, periodically treating, and sequentially carrying out precipitation treatment, freeze thawing treatment and ultraviolet irradiation treatment on the soil sample in one treatment period.
According to the simulation method for the long-term restoration of the soil heavy metals, the restoration agent is uniformly mixed with the soil to be treated, and the soil sample is subjected to periodic carbonization treatment, precipitation treatment, freeze thawing treatment and ultraviolet irradiation treatment, so that the influence of environmental factors such as acid corrosion, rainfall, cold-hot alternation and sunlight irradiation in a natural environment on the restoration effect of the restoration agent on the soil is simulated, and the treatment effect of the restoration agent under the natural condition can be simulated by comparing the leaching concentration of the heavy metals of the soil sample before and after the treatment. According to experimental data, the aging failure speed of the repairing agent on the soil sample repairing effect is 15 times of that of the same repairing agent on the soil sample under natural conditions, so that the long-term repairing simulation method for the heavy metal in the soil can effectively predict the failure rule of the repairing agent for stabilizing the effect of anions and cations under the natural environment, reduce the workload and improve the working efficiency.
In one embodiment, the soil to be detected contains at least one of cadmium, lead, chromium, arsenic, nickel and zinc, the organic carbon content of the soil to be detected is less than 1.5%, and the porosity of the soil to be detected is 25% -40%;
and/or the sampling depth of the soil to be detected is 0 cm-50 cm.
In one embodiment, in the step S3, the carbonization process includes the steps of:
and setting the carbon dioxide concentration of the experimental environment according to the sampling depth of the soil to be detected, wherein the larger the sampling depth of the soil to be detected is, the higher the carbon dioxide concentration is.
In one embodiment, the step S2 includes the following steps:
spreading the soil sample in a soil container, wherein the soil container is square or cylindrical in shape, the height of the soil container is less than 6cm, and the spreading thickness of the soil sample is 1 cm-5 cm;
the soil container is placed in the experimental environment.
In one embodiment, in the step S3, the precipitation treatment includes the steps of:
controlling the temperature of the experimental environment to be 20-25 ℃ and spraying pure water on the soil sample;
The flow rate of the spraying is determined according to the infiltration rate of the soil sample and the bottom area of the soil container, the larger the infiltration rate of the soil sample is, the larger the flow rate of the spraying is, and the larger the bottom area of the soil container is, the larger the flow rate of the spraying is;
the time of spraying is determined according to the pore volume of the soil sample and the flow rate of spraying, the larger the pore volume of the soil sample is, the longer the time of spraying is, and the larger the flow rate of spraying is, the shorter the time of spraying is.
In one of the embodiments of the present invention,
the flow rate of the sprayed pure water is Q ml/min,
the bottom area of the soil container is A cm 2 The infiltration rate of the soil sample is I mm/h;
the time for spraying the precipitation is t min,
the bottom area of the soil container is A cm 2 The tiling thickness of the soil sample is h cm, the porosity of the soil sample is n, the pore volume of the soil sample is Axh x n, and the flow of the spray precipitation is Q ml/min.
In one embodiment, before the step S1, the method further includes the following steps: drying and sieving the soil to be detected to ensure that the humidity of the soil to be detected is less than 1%, and the granularity of the soil to be detected is less than 2mm;
And/or the mixing mass ratio of the repairing agent to the soil to be detected is 1:100-1:20.
In one embodiment, in the step S3, the freeze-thawing process includes the steps of:
sequentially carrying out cooling, constant temperature, heating and cooling treatment on the temperature of the experimental environment;
the initial temperature of the freeze thawing treatment is the experimental environment temperature of the precipitation treatment, the final temperature of the freeze thawing treatment is the experimental environment temperature of the ultraviolet irradiation treatment, the temperature range of the experimental environment in the freeze thawing treatment process is-35-60 ℃, the cooling rate of the freeze thawing treatment is 8.3-10 ℃/h, and the heating rate of the freeze thawing treatment is 14.2-15.8 ℃/h.
In one embodiment, in the step S3, the ultraviolet irradiation process includes the steps of:
irradiating the surface of the soil sample with ultraviolet light with light intensity of 65-120W/m 2 The temperature of the experimental environment in the ultraviolet irradiation treatment process is 20-25 ℃.
In one embodiment, the duration of one period of the treatment period is T, T is greater than or equal to 24h, the treatment time of the carbonization treatment is T, the time of the precipitation treatment is 1/12T, the time of the freeze thawing treatment is 5/6T, and the time of the ultraviolet irradiation treatment is 1/12T.
Drawings
FIG. 1 is a flow chart of a method for detecting soil heavy metal long-term remediation in an embodiment;
FIG. 2 is a flow chart of a method for detecting soil heavy metal long-term remediation in another embodiment;
FIG. 3 is a bar graph of arsenic ion leaching concentration in soil after remediation of sample 1 and sample 2;
FIG. 4 is a bar graph of cadmium ion leach concentration in soil after remediation of sample 1 and sample 2;
FIG. 5 is a bar graph of lead ion leaching concentration in soil after remediation of sample 1 and sample 2;
FIG. 6 is a bar graph of arsenic ion leaching concentration in soil after remediation of sample 3 and sample 4;
FIG. 7 is a bar graph of cadmium ion leach concentration in soil after remediation of sample 3 and sample 4;
FIG. 8 is a bar graph of lead ion leaching concentration in soil after remediation of sample 3 and sample 4;
FIG. 9 is a bar graph of arsenic ion leaching concentration in soil after remediation of sample 3 and comparative example 1;
FIG. 10 is a bar graph of cadmium ion leaching concentration in soil after remediation of sample 3 and comparative example 1;
FIG. 11 is a bar graph of lead ion leaching concentration in soil after remediation of sample 3 and comparative example 1;
FIG. 12 is a bar graph of arsenic ion leaching concentration in soil after remediation of sample 3 and comparative example 2;
FIG. 13 is a bar graph of cadmium ion leach concentration in soil after remediation of sample 3 and comparative example 2;
FIG. 14 is a bar graph of lead ion leaching concentration in soil after remediation of sample 3 and comparative example 2;
FIG. 15 is a bar graph of arsenic ion leaching concentration in soil after remediation of sample 3 and comparative example 3, comparative example 4;
FIG. 16 is a bar graph of cadmium ion leaching concentration in soil after remediation of sample 3 and comparative example 3, comparative example 4;
FIG. 17 is a bar graph of lead ion leaching concentration in soil after remediation of sample 3 and comparative example 3, comparative example 4;
FIG. 18 is a bar graph of arsenic ion leaching concentrations in soil after remediation of sample 3 and comparative example 5;
FIG. 19 is a bar graph of cadmium ion leaching concentration in soil after remediation of sample 3 and comparative example 5;
FIG. 20 is a bar graph of lead ion leaching concentration in soil after remediation of sample 3 and comparative example 5;
FIG. 21 is a bar graph of arsenic ion leaching concentrations in soil after remediation of sample 3 and comparative example 6;
FIG. 22 is a bar graph of cadmium ion leach concentration in soil after remediation of sample 3 and comparative example 6;
FIG. 23 is a bar graph of lead ion leaching concentration in soil after remediation of sample 3 and comparative example 6;
FIG. 24 is a bar graph of arsenic ion leaching concentrations in soil after remediation of sample 3 and comparative example 7;
FIG. 25 is a bar graph of cadmium ion leach concentration in soil after remediation of sample 3 and comparative example 7;
FIG. 26 is a bar graph of lead ion leaching concentration in soil after remediation of sample 3 and comparative example 7;
FIG. 27 is a bar graph of arsenic ion leaching concentrations in soil after remediation of sample 3 and comparative example 8;
FIG. 28 is a bar graph of cadmium ion leach concentration in soil after remediation of sample 3 and comparative example 8;
fig. 29 is a bar graph of lead ion leaching concentration in soil after remediation of sample 3 and comparative example 8.
Detailed Description
In order that the above objects, features and advantages of the invention will be readily understood, a more particular description of the invention will be rendered by reference to the appended drawings. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. The present invention may be embodied in many other forms than described herein and similarly modified by those skilled in the art without departing from the spirit of the invention, whereby the invention is not limited to the specific embodiments disclosed below.
The soil heavy metal long-term restoration detection method provided by some embodiments of the present application is described in detail below.
As shown in fig. 1, in an embodiment, a method for detecting soil heavy metal long-term restoration is provided, which includes the following steps:
s1: uniformly mixing the repairing agent with soil to be detected to prepare a soil sample;
S2: placing the soil sample in an experimental environment;
s3: and carbonizing the soil sample, periodically treating, and sequentially carrying out precipitation treatment, freeze thawing treatment and ultraviolet irradiation treatment on the soil sample in one treatment period.
According to the simulation method for the long-term restoration of the soil heavy metals, the restoration agent is uniformly mixed with the soil to be treated, and the soil sample is subjected to periodic carbonization treatment, precipitation treatment, freeze thawing treatment and ultraviolet irradiation treatment, so that the influence of environmental factors such as acid corrosion, rainfall, cold-hot alternation and sunlight irradiation in a natural environment on the restoration effect of the restoration agent on the soil is simulated, and the treatment effect of the restoration agent under the natural condition can be detected by comparing the heavy metal solubility of the soil sample before and after the treatment. According to experimental data, the aging failure speed of the repairing agent on the soil sample repairing effect in the experimental environment is 15 times of that of the same repairing agent on the soil sample repairing effect in the natural condition, so that the long-term repairing simulation method for the soil heavy metals can effectively predict the failure rule of the repairing agent for stabilizing the anion and cation effects in the natural environment, reduce the workload and improve the working efficiency.
Specifically, as shown in fig. 2, in an embodiment, before the step S1, the method further includes the following steps:
and selecting a soil area polluted by heavy metals, and selecting the soil to be detected in the soil area.
Specifically, in an embodiment, the soil to be detected contains at least one of cadmium, lead, arsenic, chromium, nickel and zinc, the organic carbon content of the soil to be detected is less than 1.5%, and the porosity of the soil to be detected is 25% -40%. The acid etching effect, the rainfall scouring effect, the freeze thawing and bursting effect and the ultraviolet catalytic effect are main factors influencing the stabilization of heavy metal anions and heavy metal cations, and the method can simulate the influence of the factors on the restoration effect under natural conditions through carbonization treatment, precipitation treatment, freeze thawing treatment and ultraviolet irradiation treatment. Therefore, the soil heavy metal long-term restoration simulation method can evaluate the restoration effect of the restoration agent on various heavy metals, including heavy metal anions and heavy metal cations. The organic carbon content in the soil is more than or equal to 1.5%, so that the dissolution content of organic matters is high, and the stabilization effect of the repairing agent is affected, therefore, the soil with the organic carbon content lower than 1.5% is selected, the repairing effect of the repairing agent is more objectively evaluated, and the evaluating accuracy of the repairing agent is improved. The too large or too small porosity of the soil sample affects the stabilization effect of the restoration agent, so the porosity of the soil sample is selected to be 25% -40%.
More specifically, in one embodiment, the contents of heavy metals cadmium, lead, arsenic, chromium, nickel and zinc in the soil are all greater than the risk screening value in the soil pollution risk management and control Standard (trial) for construction of soil environmental quality (GB 36600-2018). If the concentration of heavy metal arsenic is more than 20mg/kg, the concentration of heavy metal cadmium is more than 20mg/kg, and the concentration of heavy metal lead is more than 400mg/kg.
Specifically, in one embodiment, the sampling depth of the soil to be detected is 0 cm-50 cm. In natural environment, the acid etching effect, the rainfall scouring effect, the freeze thawing collapse effect and the ultraviolet catalysis effect have the greatest influence on the shallow soil restoration effect of the restoration agent, so that the sampling depth of a selected soil area is 0 cm-50 cm, the simulation effect on the soil restoration in natural conditions is more accurate, and the actual restoration performance of the restoration agent detected by the detection method is more accurate.
Further specifically, in one embodiment, the single sample of soil to be treated is 200g to 500g. According to the technical guidelines for pollution land risk management and soil remediation effect evaluation (HJ 25.5-2018), the volume of the soil area represented by each sampling point is less than 500m 3 。
Specifically, as shown in fig. 2, in an embodiment, in the step S3, the carbonization process includes the steps of:
And setting the carbon dioxide concentration of the experimental environment according to the sampling depth of the soil to be detected, wherein the larger the sampling depth of the soil to be detected is, the higher the carbon dioxide concentration is.
Further specifically, in one embodiment, the concentration of carbon dioxide is y, y=24x+300, x is the sampling depth of the soil region, and the concentration of carbon dioxide is 300ppm to 15000ppm. In natural environment, the carbon dioxide concentration in the atmosphere is 300ppm, and the carbon dioxide concentration in deep soil is 15000ppm, so that the method simulates the shallow soil of natural environment, the carbon dioxide concentration of the shallow soil is 300 ppm-15000 ppm, and the carbon dioxide concentration of soil areas with different depths is tested to obtain the linear function relation of the carbon dioxide concentration and the sampling depth of the soil areas.
Specifically, as shown in fig. 2, in an embodiment, the step S2 includes the following steps:
spreading the soil sample in a soil container, wherein the soil container is square or cylindrical in shape, the height of the soil container is less than 6cm, and the spreading thickness of the soil sample is 1 cm-5 cm;
the soil container is placed in the experimental environment.
The soil container is too high, and the light path of ultraviolet irradiation treatment can be shielded, so that the surface of the soil sample is not uniformly irradiated with ultraviolet. Too large thickness of the soil sample can cause poor illumination uniformity of ultraviolet irradiation in the thickness direction of the soil sample, thereby affecting the accuracy of the repair effect evaluation. Meanwhile, the soil sample is too low in thickness, so that the soil splashes in the rainfall treatment process.
Specifically, as shown in fig. 2, in an embodiment, in the step S3, the precipitation treatment includes the following steps:
controlling the temperature of the experimental environment to be 20-25 ℃ and spraying pure water on the soil sample;
the flow rate of the spraying is determined according to the infiltration rate of the soil sample and the bottom area of the soil container, the larger the infiltration rate of the soil sample is, the larger the flow rate of the spraying is, and the larger the bottom area of the soil container is, the larger the flow rate of the spraying is;
the time of spraying is determined according to the pore volume of the soil sample and the flow rate of spraying, the larger the pore volume of the soil sample is, the longer the time of spraying is, and the larger the flow rate of spraying is, the shorter the time of spraying is.
Specifically, in one embodiment, the flow rate of the sprayed pure water is Q ml/min,
the bottom area of the soil container is A cm 2 The infiltration rate of the soil sample is I mm/h;
the time for spraying the precipitation is t min,
the bottom area of the soil container is A cm 2 The tiling thickness of the soil sample is h cm, the porosity of the soil sample is n, the pore volume of the soil sample is Axh x n, and the flow of the spray precipitation is Q ml/min.
Specifically, as shown in fig. 2, in an embodiment, before the step S1, the method further includes the following steps: and drying and sieving the soil to be detected to ensure that the humidity of the soil to be detected is less than 1%, and the granularity of the soil to be detected is less than 2mm. The soil to be treated is dried and screened, so that the humidity and granularity of the soil are further regulated, and irrelevant variables for evaluating the repairing effect are controlled.
Specifically, in an embodiment, the mixing mass ratio of the repairing agent to the soil to be detected is 1:100-1:20. The mixing mass ratio of the repairing agent and the soil to be treated enables the repairing agent to be completely mixed with the soil to be treated, and the treatment effect is best.
Specifically, in an embodiment, in the step S3, the freeze-thawing process includes the steps of:
sequentially carrying out cooling, constant temperature, heating and cooling treatment on the temperature of the experimental environment;
the initial temperature of the freeze thawing treatment is the experimental environment temperature of the precipitation treatment, the final temperature of the freeze thawing treatment is the experimental environment temperature of the ultraviolet irradiation treatment, the temperature range of the experimental environment in the freeze thawing treatment process is-35-60 ℃, the cooling rate of the freeze thawing treatment is 8.3-10 ℃/h, and the heating rate of the freeze thawing treatment is 14.2-15.8 ℃/h.
The temperature range of the freeze thawing treatment is determined according to the highest temperature and the lowest temperature in the natural environment. In the freezing and thawing treatment process, the temperature rising rate and the temperature reducing rate cannot be too fast, the condition that a soil sample is quenched or suddenly heated is avoided, the soil sample is completely disintegrated to lose original properties, or the soil is partially melted into slurry, so that the physical and chemical properties of the soil sample are irreversibly changed, and the properties of the soil sample are inconsistent with those of the soil sample in the natural environment, and the simulation restoration result is inconsistent with the restoration result in the natural environment.
Specifically, in an embodiment, in the step S3, the ultraviolet irradiation process includes the steps of:
irradiating the surface of the soil sample with ultraviolet light with light intensity of 65-120W/m 2 The temperature of the experimental environment in the ultraviolet irradiation treatment process is 20-25 ℃. The intensity of ultraviolet irradiation treatment is determined according to the intensity of ultraviolet light in the high latitude areas of the Tibetan of China, and is the strongest illumination intensity of China. If the repairing agent can ensure good stabilizing effect under the strongest ultraviolet irradiation, it can be estimated that the repairing agent can still maintain good stabilizing effect under weaker conditions.
Specifically, in an embodiment, the duration of one period of the treatment period is T, T is greater than or equal to 24h, the treatment time of the carbonization treatment is T, the time of the precipitation treatment is 1/12T, the time of the freeze thawing treatment is 5/6T, and the time of the ultraviolet irradiation treatment is 1/12T.
Further specifically, in one embodiment, the treatment period is 24 hours for simulating a restoration environment of the soil sample within 15 days under natural conditions. The treatment time of carbonization treatment is 24 hours, the time of precipitation treatment is 2 hours, the time of freeze thawing treatment is 20 hours, and the time of ultraviolet irradiation treatment is 2 hours. Thus, during the test, depending on the healing effect of the healing agent under natural conditions within a certain period of time, a suitable treatment cycle is selected, or a suitable number of treatment cycles is selected. For example, when the restoration effect of the restoration agent within 1 month needs to be tested, two treatment cycles (24 h) can be performed on the soil sample, namely, the restoration effect of the soil sample in the two treatment cycles is consistent with the restoration effect of the soil in the natural environment for one month.
Specifically, in an embodiment, the sample 1 adopts the soil heavy metal long-term restoration detection method in the application, and specific parameters are as follows:
step one: selecting an industrial polluted soil area containing arsenic, cadmium and lead, wherein the organic carbon content of the soil area is 0.7%, the porosity of the soil area is 31%, the arsenic concentration is 22mg/kg, the cadmium concentration is 30mg/kg, and the lead concentration is 871mg/kg, the sampling depth of the soil area is 20cm, the sampling amount of the soil to be treated is 400g, and the representative volume of the soil area is 500m 3 ；
Step two: drying the taken soil to be treated at 40 ℃, and sieving the soil by a 100-mesh sieve to ensure that the humidity of the soil to be treated is 1%, wherein the granularity of the soil to be treated is 2mm;
step three: uniformly mixing soil to be treated with 3% goethite restoration agent to obtain a soil sample; the soil sample is put into a plastic square soil container with the side length of 5cm and the height of 4cm, and the spreading thickness of the soil sample is 3cm;
step four: and (3) carrying out 12-cycle treatment on the soil sample in 24 hours of one treatment cycle, and respectively testing the leaching concentration of arsenic ions, cadmium ions and lead ions of the sample 1 in the 2 nd, 4 th, 6 th, 8 th, 10 th and 12 th treatment cycles.
Within one processing cycle 24 h:
carbonizing: the concentration of carbon dioxide is 780ppm, and the treatment time is 0-24 h;
precipitation treatment: the precipitation temperature is 25 ℃, the spraying rate is 1.7ml/min, the spraying time is 42.9min, and the treatment time is 0-2 h;
and (3) freezing and thawing treatment: cooling to-35 ℃ for 2-8 h, wherein the cooling rate is 10 ℃/h; 8-14 h, and keeping the temperature at-35 ℃; the temperature is increased to 60 ℃ for 14 to 20 hours, and the temperature rising rate is 15.8 ℃/h; the temperature is reduced to 20 ℃ for 20-22 hours, and the cooling rate is 20 ℃/h;
ultraviolet irradiation treatment: the light intensity of the ultraviolet irradiation treatment was 120W/m 2 The environmental temperature of the ultraviolet irradiation treatment is 20 ℃, and the treatment time is 22-24 hours.
Wherein, sample 1 is the same with sample 2 sample soil region, the same kind of restoration agent, the mixing ratio of restoration agent and soil sample, sample depth are the same, sample 2's treatment process is as follows:
step one: the soil sampling area is the same as the sample 1, the soil 2 to be detected is taken in the area, and the soil 2 to be detected and the repairing agent are uniformly mixed to obtain a soil sample 2;
step two: adding 30% pure water into the soil sample 2, and standing for 7 days;
step three: filling the soil sample 2 into the original sampling area, sampling at the time of repairing 1 st, 2 nd, 3 rd, 4 th, 5 th and 6 th months respectively, and testing the leaching concentration of arsenic ions, cadmium ions and lead ions of the soil sample 2.
Similarly, as shown in fig. 4, the aging failure rate of the repair effect of the same cadmium ion in the experimental environment is 15 times that of the repair effect in the natural environment, which is a histogram of the leaching concentration of the cadmium ion in the soil after repair by the repair agent in the natural environment (sample 1) and the experimental environment (sample 2). As shown in fig. 5, a bar graph of lead ion leaching concentration in soil after remediation by a remediation agent in a natural environment (sample 1) and an experimental environment (sample 2). The aging failure speed of the repair effect of the same lead ions in the experimental environment is 15 times of that of the repair effect in the natural environment. Therefore, the soil heavy metal long-term restoration detection method can effectively predict the failure rule of the effect of stabilizing anions and cations by the restoration agent in natural environment, reduce the workload and improve the working efficiency.
In another embodiment, the sample 3 adopts the soil heavy metal long-term restoration detection method in the application, and specific parameters are as follows:
step one: selecting an industrial polluted soil area containing arsenic, cadmium and lead, wherein the organic carbon content of the soil area is 12% of the soil area, wherein the porosity of the soil area is 42%, the arsenic concentration is 75mg/kg, the cadmium concentration is 36mg/kg, the lead concentration is 450mg/kg, the sampling depth of the soil area is 50cm, the sampling amount of the soil to be treated is 200g, and the representative volume of the soil area is 500m 3 ；
Step two: drying the taken soil to be treated at 40 ℃, and sieving the soil by a 100-mesh sieve to ensure that the humidity of the soil to be treated is 1%, wherein the granularity of the soil to be treated is 2mm;
step three: uniformly mixing soil to be treated with 5% reduced iron powder (repairing agent) to obtain a soil sample; the soil sample is filled into a plastic cylindrical soil container with the diameter of 5cm and the height of 6cm, and the spreading thickness of the soil sample is 5cm;
step four: and (3) carrying out 12-cycle treatment on the soil sample in 24 hours of one treatment cycle, and respectively testing the leaching concentration of arsenic ions, cadmium ions and lead ions of the sample 3 in the 2 nd, 4 th, 6 th, 8 th, 10 th and 12 th treatment cycles.
Within one processing cycle 24 h:
carbonizing: the concentration of carbon dioxide is 1500ppm, and the treatment time is 0-24 h;
precipitation treatment: the precipitation temperature is 22 ℃, the spraying rate is 3.67ml/min, the spraying time is 45min, and the treatment time is 0-2 h;
and (3) freezing and thawing treatment: cooling to-32 ℃ for 2-8 h, wherein the cooling rate is 8.33 ℃/h; 8-14 h, and keeping the temperature at-32 ℃; the temperature is increased to 60 ℃ for 14 to 20 hours, and the temperature rising rate is 15.3 ℃/h; the temperature is reduced to 22 ℃ for 20-22 hours, and the cooling rate is 19 ℃/h;
Ultraviolet irradiation treatment: the light intensity of the ultraviolet irradiation treatment is 65W/m 2 The environment temperature of the ultraviolet irradiation treatment is 22 ℃, and the treatment time is 22-24 hours.
step one: the sampling soil area is the same as the sample 3, the soil 4 to be detected is taken in the area, and the soil 4 to be detected and the repairing agent (reduced iron powder) are uniformly mixed to obtain a soil sample 4;
step two: adding 30% pure water into the soil sample 4, and standing for 7 days;
step three: filling the soil sample 4 into the original sampling area, sampling at the time of repairing 1 st, 2 nd, 3 rd, 4 th, 5 th and 6 th months respectively, and testing the leaching concentration of arsenic ions, cadmium ions and lead ions of the soil sample 4.
Therefore, as can be seen from fig. 6, 7 and 8, when the repair effect of the repair agent on arsenic ions, cadmium ions and lead ions is the same, the repair time in the natural environment (sample 4) is 15 times longer than that in the experimental environment (sample 3). The soil heavy metal long-term restoration detection method can effectively predict the failure rule of the effect of stabilizing anions and cations by the restoration agent in natural environment, reduce the workload and improve the working efficiency.
In yet another example, comparative examples 1-7 were each treated with the soil heavy metal long term remediation test method of the present application. The treatment conditions of comparative examples 1 to 7 and sample 3 are shown in Table 1, and the other treatment parameters of comparative examples 1 to 7 and sample 3 are the same except for the parameters in Table 1.
Specifically, comparative example 1 increased the organic carbon content (2.5%) of the soil to be detected as compared with the treatment process of sample 3, other treatment parameters were the same as those of sample 3, and the treatment results of sample 3 and comparative example 1 were compared to obtain fig. 9, 10 and 11. As can be seen from fig. 9, 10 and 11, the arsenic ion concentration of comparative example 1 after repair is significantly increased compared with sample 3, and the concentration change of cadmium ion and lead ion is not obvious, which indicates that the excessive organic carbon content may cause the effect of repairing arsenic ion by the repairing agent to be worse in experimental environment than in natural environment. The method is characterized in that the arsenic ions have strong affinity with organic matters in soil, and the high-concentration organic matters can accelerate the dissolution of soluble organic carbon, so that the repairing effect of the repairing agent in the experimental environment is obviously different from the aging failure rule and the natural environment. Therefore, the organic carbon concentration of the soil to be detected selected by the soil heavy metal long-term restoration detection method is required to be lower than 1.5%, so that the accuracy of the anion treatment effect in the soil can be ensured.
Specifically, comparative example 2 changed the treatment sequence of the soil sample (ultraviolet irradiation treatment followed by precipitation treatment and freeze thawing treatment) as compared with the treatment process of sample 3, and other treatment parameters were the same as those of sample 3, and the treatment results of sample 3 and comparative example 2 were compared to obtain fig. 12, 13 and 14. As can be seen from fig. 12, 13 and 14, the heavy metal concentrations of arsenic ions, cadmium ions and lead ions are significantly reduced, and the treatment effect from sample 3 is significantly different, that is, from that in the natural environment. This is because the main reason why the material stabilization effect is lost due to ultraviolet irradiation is that the material-heavy metal system is attacked by free radicals, and the physical shielding shadow effect of soil minerals is the most dominant mechanism against this attack; the effect of the carbonization treatment is not significant in the range of 0 to 2 hours, resulting in that the soil mineral without allosteric shade the material-heavy metal system from oxidation by free radicals generated by uv ageing. However, the carbonization treatment is carried out for 22-24 hours, so that the deformation of soil minerals is gradually remarkable, the shielding effect of the minerals on free radicals is gradually weakened, and the free radicals generated by ultraviolet can directly and effectively attack a material-heavy metal system. Therefore, in the method for detecting the long-term restoration of the heavy metal in the soil, precipitation treatment, freeze thawing treatment and ultraviolet treatment are needed to be sequentially carried out, so that the same restoration effect aging failure rule as that in the natural environment can be achieved, and the accuracy of the detection of the restoration effect of the restoration agent is ensured.
Specifically, comparative example 3, comparative example 4 changed the ultraviolet intensity compared to the treatment process of sample 3The other processing parameters were the same as those of sample 3, and the processing results of sample 3 and comparative examples 3 and 4 were compared to obtain fig. 15, 16 and 17. As can be seen from FIGS. 15, 16 and 17, the ultraviolet light was set to 40W/m in comparative example 3 2 (below 65W/m) 2 ) The heavy metal concentrations of arsenic ions, cadmium ions and lead ions after repair are obviously reduced, and the concentration of ultraviolet light is 130W/m in comparative example 4 2 (greater than 120W/m) 2 ) The concentration of heavy metals of arsenic ions, cadmium ions and lead ions after repair is obviously increased, and the difference between the heavy metal concentration and the treatment effect of the sample 3 is obvious, namely the treatment effect in natural environment is obvious. Therefore, the concentration of the ultraviolet light must be 65W/m during the ultraviolet treatment 2 ～120W/m 2 And the accuracy of the accelerated prediction simulation of the repairing effect of the repairing agent in the laboratory is ensured.
Specifically, comparative example 5 increased the tile thickness of the soil sample compared to the treatment process of sample 3, other treatment parameters were the same as sample 3, and the treatment results of sample 3 and comparative example 5 were compared to obtain fig. 18, 19 and 20. As can be seen from fig. 18, 19 and 20, comparative example 5 sets the tile thickness of the soil sample to 6cm (more than 5 cm), and the heavy metal concentrations of arsenic ions, cadmium ions and lead ions after repair are significantly reduced, and the difference in treatment effect from sample 3, that is, the difference in treatment effect from the natural environment is significant. Because the thickness of ultraviolet irradiation can only be less than 5cm, in the method for long-term repair and detection of soil heavy metals, the tiled thickness of a soil sample is less than 5cm, and the accuracy of the repair effect detection of the repairing agent is higher.
Specifically, comparative example 6 shortens the time of carbonization treatment compared with the treatment process of sample 3, other treatment parameters are the same as sample 3, and comparison of the treatment results of sample 3 and comparative example 6 gives fig. 21, 22 and 23. As can be seen from fig. 21, 22 and 23, comparative example 6 was set to have a carbonization treatment time of 12 hours in one cycle, and the heavy metal concentrations of arsenic ions, cadmium ions and lead ions after repair were significantly reduced, and the treatment effect difference from that of sample 3, that is, the treatment effect difference from that in the natural environment was significant. Therefore, the carbonization repair time is important, and the detection accuracy is seriously affected.
Specifically, comparative example 7 changed the rate of decrease and the rate of increase in the temperature of the freeze-thawing treatment compared to the treatment process of sample 3, so that the freeze-thawing treatment of comparative example 7 was insufficient, other treatment parameters were the same as those of sample 3, and the treatment results of sample 3 and comparative example 5 were compared, resulting in fig. 24, 25 and 26. As can be seen from fig. 24, 25 and 26, the freeze-thawing treatment operation is set in comparative example 7 as follows: 2-8 h: cooling to-25 ℃, wherein the cooling rate is 7.83 ℃/h; 8-14 h: constant temperature at-25 ℃; 14-20 h: the temperature is increased to 60 ℃ and the temperature rising rate is 14.2 ℃/h; 20-22 h: the temperature is reduced to 22 ℃ and the cooling rate is 19 ℃/h; the freezing and thawing cooling rate is too low, the heating rate is too high, the freezing and thawing is insufficient, the concentration of heavy metals of arsenic ions, cadmium ions and lead ions after repair is obviously reduced, and the difference between the heavy metals and the treatment effect of the sample 3 is obvious, namely the difference between the heavy metals and the treatment effect in the natural environment is obvious.
Specifically, comparative example 8 changed the rate of decrease and the rate of increase of the freezing and thawing treatment compared to the treatment process of sample 3, so that comparative example 8 was excessively frozen and thawing treatment, other treatment parameters were the same as sample 3, and the treatment results of sample 3 and comparative example 8 were compared, resulting in fig. 27, fig. 28 and fig. 29. As can be seen from fig. 27, 28 and 29, the freeze-thawing treatment operation is set in comparative example 8 as follows: 2-8 h: cooling to-40 ℃, wherein the cooling rate is 10.33 ℃/h; 8-14 h: constant temperature at-40 ℃; 14-20 h: the temperature is increased to 60 ℃ and the heating rate is 16.7 ℃/h; 20-22 h: the temperature is reduced to 22 ℃ and the cooling rate is 19 ℃/h; the freezing and thawing cooling rate is too high, the heating rate is too high, the freezing and thawing is excessive, the concentration of heavy metals of arsenic ions, cadmium ions and lead ions after repair is obviously increased, and the difference between the heavy metals and the treatment effect of the sample 3 is obvious, namely the difference between the heavy metals and the treatment effect in the natural environment is obvious. Therefore, in the freezing and thawing treatment process, the cooling rate should be kept at 8.3 ℃/h to 10 ℃/h, and the heating rate should be kept at 14.2 ℃/h to 15.8 ℃/h, so that the detection result is more accurate.
Table 1: comparative examples 1-8 were compared to the treatment conditions of sample 3;
in the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element being referred to must have a specific orientation, be configured and operated in a specific orientation, and therefore should not be construed as limiting the present invention.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include at least one such feature. In the description of the present invention, the meaning of "plurality" means at least two, for example, two, three, etc., unless specifically defined otherwise.
In the present invention, unless explicitly specified and limited otherwise, the terms "mounted," "connected," "secured," and the like are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; either directly or indirectly, through intermediaries, or both, may be in communication with each other or in interaction with each other, unless expressly defined otherwise. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances.
In the present invention, unless expressly stated or limited otherwise, a first feature "up" or "down" a second feature may be the first and second features in direct contact, or the first and second features in indirect contact via an intervening medium. Moreover, a first feature being "above," "over" and "on" a second feature may be a first feature being directly above or obliquely above the second feature, or simply indicating that the first feature is level higher than the second feature. The first feature being "under", "below" and "beneath" the second feature may be the first feature being directly under or obliquely below the second feature, or simply indicating that the first feature is less level than the second feature.
It will be understood that when an element is referred to as being "fixed" or "disposed" on another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. The terms "vertical," "horizontal," "upper," "lower," "left," "right," and the like are used herein for illustrative purposes only and are not meant to be the only embodiment.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (10)
1. The method for detecting the long-term restoration of the heavy metals in the soil is characterized by comprising the following steps of:
s1: uniformly mixing a repairing agent with soil to be detected to prepare a soil sample, wherein the organic carbon content of the soil to be detected is less than 1.5%;
s2: placing the soil sample in an experimental environment, wherein the laying thickness of the soil sample is 1 cm-5 cm;
s3: carbonizing the soil sample, periodically treating, and sequentially carrying out precipitation treatment, freeze thawing treatment and ultraviolet irradiation treatment on the soil sample in a treatment period; the cooling rate of the freeze thawing treatment is 8.3-10 ℃/h, and the heating rate of the freeze thawing treatment is 14.2-15.8 ℃/h; the light intensity of the ultraviolet light of the ultraviolet irradiation treatment is 65-120W/m 2 。
2. The method for long-term remediation and detection of heavy metals in soil according to claim 1, wherein the soil to be detected contains at least one of cadmium, lead, arsenic, chromium, nickel and zinc, and the porosity of the soil to be detected is 25% -40%;
and/or the sampling depth of the soil to be detected is 0 cm-50 cm.
3. The method according to claim 1, wherein in the step S3, the carbonization treatment comprises the steps of:
And setting the carbon dioxide concentration of the experimental environment according to the sampling depth of the soil to be detected, wherein the larger the sampling depth of the soil to be detected is, the higher the carbon dioxide concentration is.
4. The method for long-term soil heavy metal remediation detection according to claim 1, wherein the step S2 includes the steps of:
spreading the soil sample in a soil container, wherein the soil container is square or cylindrical in shape, and the height of the soil container is less than 6cm;
the soil container is placed in the experimental environment.
5. The method according to claim 4, wherein in the step S3, the precipitation treatment includes the steps of:
controlling the temperature of the experimental environment to be 20-25 ℃ and spraying pure water on the soil sample;
the flow rate of the spraying is determined according to the infiltration rate of the soil sample and the bottom area of the soil container, the larger the infiltration rate of the soil sample is, the larger the flow rate of the spraying is, and the larger the bottom area of the soil container is, the larger the flow rate of the spraying is;
the time of spraying is determined according to the pore volume of the soil sample and the flow rate of spraying, the larger the pore volume of the soil sample is, the longer the time of spraying is, and the larger the flow rate of spraying is, the shorter the time of spraying is.
6. The method for long-term soil heavy metal remediation detection according to claim 5, wherein the flow rate of the sprayed pure water is Q ml/min,
the bottom area of the soil container is A cm 2 The infiltration rate of the soil sample is I mm/h;
the time for spraying the precipitation is t min,
the bottom area of the soil container is A cm 2 The tiling thickness of the soil sample is h cm, the porosity of the soil sample is n, the pore volume of the soil sample is Axh x n, and the flow of the spray precipitation is Q ml/min.
7. The method for long-term soil heavy metal remediation detection of any one of claims 1 to 6, further comprising, prior to step S1, the steps of: drying and sieving the soil to be detected to ensure that the humidity of the soil to be detected is less than 1%, and the granularity of the soil to be detected is less than 2mm;
and/or the mixing mass ratio of the repairing agent to the soil to be detected is 1:100-1:20.
8. The method for long-term soil heavy metal remediation detection of any one of claims 1 to 6, wherein in step S3, the freeze-thawing treatment includes the steps of:
sequentially carrying out cooling, constant temperature, heating and cooling treatment on the temperature of the experimental environment;
The initial temperature of the freeze thawing treatment is the experimental environment temperature of the precipitation treatment, the final temperature of the freeze thawing treatment is the experimental environment temperature of the ultraviolet irradiation treatment, and the temperature range of the experimental environment in the freeze thawing treatment process is-35-60 ℃.
9. The method for long-term soil heavy metal remediation detection of any one of claims 1 to 6, wherein in step S3, the ultraviolet radiation treatment includes the steps of:
and irradiating the surface of the soil sample by ultraviolet light, wherein the temperature of the experimental environment is 20-25 ℃ in the ultraviolet irradiation treatment process.
10. The method for long-term soil heavy metal remediation detection according to any one of claims 1 to 6, wherein the duration of one cycle of the treatment cycle is T, T is 24 hours or more, the treatment time of the carbonization treatment is T, the time of the precipitation treatment is 1/12T, the time of the freeze thawing treatment is 5/6T, and the time of the ultraviolet irradiation treatment is 1/12T.
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Application publication date: 20220624 Assignee: Nanjing Qingke Zhongsheng Environmental Protection Materials Co.,Ltd. Assignor: TSINGHUA University Contract record no.: X2023980044874 Denomination of invention: Long term remediation detection method for heavy metals in soil Granted publication date: 20230512 License type: Common License Record date: 20231030 |