CN113109108A - Sampling method for obtaining soil solution by efficient online leaching - Google Patents
Sampling method for obtaining soil solution by efficient online leaching Download PDFInfo
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- CN113109108A CN113109108A CN202110330802.9A CN202110330802A CN113109108A CN 113109108 A CN113109108 A CN 113109108A CN 202110330802 A CN202110330802 A CN 202110330802A CN 113109108 A CN113109108 A CN 113109108A
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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
- 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
- G01N1/40—Concentrating samples
- G01N1/4044—Concentrating samples by chemical techniques; Digestion; Chemical decomposition
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a sampling method for obtaining soil solution by efficient online leaching, which comprises the following steps: adding borax into a sodium hydroxide solution to prepare an alkaline buffer solution; adding a chelating agent into a sodium citrate solution to obtain a mixed solution; adding a biosurfactant and an alkaline buffer solution into the mixed solution, and uniformly mixing to obtain an extractant; and mixing the leaching agent with the soil sample to be detected through a sampling device, and separating heavy metal elements in the soil sample to be detected into the leaching agent by utilizing the dipping effect of the leaching agent on the soil to obtain a soil solution. According to the sampling method provided by the invention, the leaching agent and the leaching device are improved simultaneously, so that the laboratory environment can be separated, a soil solution sample can be quickly and conveniently obtained, and the detection efficiency of heavy metal ions in soil is improved.
Description
Technical Field
The invention belongs to the technical field of environmental monitoring, and particularly relates to a sampling method for obtaining a soil solution by efficient online leaching.
Background
The heavy metal pollution of the soil refers to the condition that the content of trace metal elements in the soil exceeds a background value due to human activities and is over-high due to excessive deposition, and the condition is generally called as soil heavy metal pollution. The heavy metals in the polluted soil mainly comprise elements with obvious biological toxicity, such As mercury (Hg), cadmium (Cd), lead (Pb), chromium (Cr), metalloid arsenic (As) and the like, and elements with certain toxicity, such As zinc (Zn), copper (Cu), nickel (Ni) and the like. The heavy metal pollutants have poor mobility in soil, long retention time and can not be degraded by microorganisms; and can finally affect human health through media such as water, plants and the like. The detection of the content of heavy metal ions in soil has important significance for monitoring the soil quality, and becomes a necessary detection link in occasions such as environmental inspection, crop planting and the like.
And all detection samples of the content of heavy metal ions in the soil are soil solutions. The soil solution sample can be obtained in various ways, such as: sampling in a 'field' shape, bringing the sample into a laboratory after field sampling, sterilizing at high temperature and digesting with microwaves to obtain a soil solution sample, but the method is time-consuming and labor-consuming, needs strong acid and strong base for microwave digestion, has high technical requirements on operators and has high risk coefficient; besides, researchers can install ion exchange resin in the in-situ soil deep layer, and determine the ion concentration through long-time (>7 days) exchange and observation, and the method is suitable for long-term study of the rule of ion migration and is not suitable for the field of instant detection.
The heavy metal ion removing and leaching process includes the steps of reacting a reagent (leaching agent) with heavy metals in soil to form soluble heavy metal ions or metal complexes, and separating the heavy metals from the soil to obtain a soil solution containing the heavy metal ions. However, the existing heavy metal ion removing and leaching device is required to be carried out in a laboratory, the operation limiting conditions are more, the dosage of the required leaching agent is large, and the operation is not convenient and fast; in addition, the existing leaching reagent has low separation rate and extraction efficiency on heavy metal ions in soil, and is easy to cause secondary pollution. Therefore, how to obtain the soil solution efficiently, quickly and environmentally is an urgent technical problem to be solved.
Disclosure of Invention
The invention aims to provide a sampling method for obtaining soil solution by efficient online leaching, which can be separated from a laboratory environment, quickly and conveniently obtain a soil solution sample and improve the detection efficiency of heavy metal ions in soil by simultaneously improving two aspects of a leaching agent and a leaching device.
In order to achieve the purpose, the invention adopts the technical scheme that:
a sampling method for obtaining soil solution by efficient online leaching comprises the following steps:
adding borax into a sodium hydroxide solution to prepare an alkaline buffer solution; adding a chelating agent into a sodium citrate solution to obtain a mixed solution; adding a biosurfactant and an alkaline buffer solution into the mixed solution, and uniformly mixing to obtain an extractant; borax has the characteristics of low acidity and environmental friendliness, and the prepared alkaline buffer solution (BGS for short) can ensure stable components of a subsequent leaching agent and effectively carry out reaction; the sodium citrate is an environment-friendly complexing agent, does not cause secondary pollution after being discharged, and aims at Cu in soil2+、Ca2+、Zn2+Etc. has good complexing effect and can make up for Na2Complexation range of EDTA and in Na2Under the optimal complexing condition of EDTA, sodium citrate is one of organic acid complexing agents with the strongest complexing ability on metal;
and mixing the leaching agent with the soil sample to be detected, and separating heavy metal elements in the soil sample to be detected into the leaching agent through the soaking effect of the leaching agent on the soil to obtain a soil solution.
As a preferable technical scheme, the pH value of the alkaline buffer solution is 9-10; the chelating agent is Na2One of EDTA, DTPA, DTPMA, EDTPMA and PBTCA; the biosurfactant isOne of rhamnolipid, cellobiose, and algal glycolipid. The surfactant has hydrophilic groups and lipophilic groups, and can promote the leaching liquor and the soil colloid to fully contact and carry out complexation reaction. The rhamnolipid is the most optimal biosurfactant, and because the rhamnolipid is widely existed in natural soil, the rhamnolipid does not cause secondary pollution to the soil, and the rhamnolipid is low in production cost and suitable for batch application. Further preferably, the mass ratio of the biosurfactant to the mixed solution is 1: 1000.
As a preferable technical scheme, the method for uniformly mixing is ultrasonic oscillation. The ultrasonic oscillation is that the high-frequency sound wave of the ultrasonic wave is used for generating oscillation, the cavitation effect of the ultrasonic wave is used for quickly dissolving the solute, and the gas in the leaching liquor can be discharged.
As a preferred technical scheme, the leaching agent and the soil sample to be detected are mixed in a sampling device, the sampling device comprises a support frame, a vacuum cavity is fixed on the support frame, one end of the vacuum cavity is connected with a storage chamber and a soil sample collection box through a connecting component, and the other end of the vacuum cavity is connected with a vacuum pump through a vacuum pipeline; the connecting assembly comprises a first three-way joint, a second three-way joint and a liquid suction head;
the first end of the first three-way joint is connected with one end of the vacuum cavity through a first pipeline; the second end of the first tee joint is connected with one end of a liquid suction head through a second pipeline, and the other end of the liquid suction head is placed in a soil sample collection box; the third end of the first three-way joint is connected with the first end of the second three-way joint through a third pipeline; the second end of the second three-way joint is connected with the soil sample collection box through a fourth pipeline; the third end of the second three-way joint is connected with the storage chamber through a fifth pipeline; a first one-way valve is arranged on the second pipeline, and a second one-way valve is arranged on the third pipeline; a first electromagnetic valve is installed on the fourth pipeline, and a second electromagnetic valve is installed on the fifth pipeline;
the soil sample collection box is connected with a stirrer, and a stirring head of the stirrer extends into the soil sample collection box.
According to a preferable technical scheme, the vacuum pipeline comprises a first vacuum pipeline and a second vacuum pipeline, a third electromagnetic valve is installed on the first vacuum pipeline, and a fourth electromagnetic valve is installed on the second vacuum pipeline; one end of the first vacuum pipeline is connected with the vacuum cavity, the other end of the first vacuum pipeline is connected with the vacuum pump through a third tee joint, and a fifth electromagnetic valve is installed at the free end of the third tee joint; one end of the second vacuum pipeline is connected with the vacuum cavity, the other end of the second vacuum pipeline is connected with the vacuum pump through a fourth three-way joint, and a sixth electromagnetic valve is installed at the free end of the fourth three-way joint. Through dividing into first vacuum pipeline and second vacuum pipeline with the vacuum pipeline to set up corresponding solenoid valve, when the device was in washing operating condition, open the solenoid valve, the washing liquid can directly be discharged from third three way connection, fourth three way connection's free end, improves cleaning efficiency.
As a preferred technical scheme, a silica gel sleeve is coated outside the stirrer; the silica gel cover has certain cushioning effect, can avoid agitator and soil sample collection box direct contact through the outside cladding silica gel cover at the agitator, has certain guard action to soil sample collection box. The stirring head of the stirrer is a metal T-shaped stirring head.
As a preferred technical scheme, a battery pack for supplying power is further installed on the support frame, and the battery pack is electrically connected with the first electromagnetic valve, the second electromagnetic valve, the third electromagnetic valve, the fourth electromagnetic valve, the fifth electromagnetic valve and the sixth electromagnetic valve.
As a preferred technical scheme, the liquid suction head is a polyester film liquid suction head, and a PVC slim tube is sleeved in the polyester film liquid suction head; one end of the polyester film liquid absorption head is sealed by an AB adhesive, and the other end of the polyester film liquid absorption head is connected with a second pipeline through a luer connector. Since the polyester film is too soft, in order to improve the flexibility, a PVC thin tube is sleeved inside the polyester film, so that a linear suction head is formed. When the liquid suction head is used, the liquid suction head made of the polyester film is bent and placed at the bottom of the soil sample collection box, the liquid level is guaranteed to be completely immersed, and the use efficiency of the liquid suction head is improved.
As the preferred technical scheme, the support frame comprises a working platform and support legs vertically fixed at the bottom of the working platform. The vacuum pump adopts a Kammer 12V brushless motor vacuum pump; the vacuum cavity is columnar; the soil sample collection box is made of PVC plastic; the vacuum cavity is made of medical PP materials.
The electromagnetic valve, the one-way valve, the battery pack and the like are all commercially available products, and the specific working principle of the electromagnetic valve, the one-way valve, the battery pack and the like is not described herein in detail. The on and off of each electromagnetic valve can be controlled manually or automatically by a control system, and the two modes are conventional control modes in the field and are not described herein.
Compared with the prior art, the invention has the beneficial effects that:
through carrying out the simultaneous improvement to two aspects of lixiviant and leaching device, can break away from the laboratory environment, gain the soil solution sample fast conveniently, improve heavy metal ion detection efficiency in the soil. Compared with the traditional Na alone in the aspect of leaching agent2The EDTA lixiviant or the organic acid lixiviant has better lixiviation effect; in the aspect of the sampling device, the sampling device provided by the invention has small occupied space and is convenient to move, the solution collection can be carried out on the soil sample to be detected in situ, large-scale equipment and complex processes are not needed, the operation can be carried out by detection personnel without professional training, the operation is simple, the sampling period is short, and only 2-3 h is needed to complete one sampling operation. And the device can be recycled, and when another soil sample needs to be detected, the next sampling can be carried out after the cleaning device is cleaned.
Drawings
FIG. 1 is a first schematic view of a sampling device used in the present invention;
FIG. 2 is a second schematic structural view of a sampling device used in the present invention;
reference numerals: 1-support frame, 11-working platform, 12-support leg, 2-vacuum cavity, 31-first three-way joint, 311-first pipeline, 312-second pipeline, 313-third pipeline, 32-second three-way joint, 321-fourth pipeline, 322-fifth pipeline, 33-liquid suction head, 34-first one-way valve, 35-second one-way valve, 36-first solenoid valve, 37-second solenoid valve, 4-storage chamber, 5-soil sample collection box, 6-vacuum pump, 7-stirrer, 81-first vacuum pipeline, 82-second vacuum pipeline, 83-third solenoid valve, 84-fourth solenoid valve, 9-third three-way joint, 10-fifth solenoid valve, 11-fourth three-way joint, 12-a sixth electromagnetic valve, 13-a silica gel sleeve, 14-a control system, 15-a battery pack and 16-a luer connector.
Detailed Description
The invention is further described with reference to the following figures and examples. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the present invention, unless otherwise expressly specified or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can include, for example, fixed connections, removable connections, or integral connections; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
It is to be understood that the terms "upper," "lower," "left," "right," "top," "bottom," "inner," "outer," and the like are used in the orientations and positional relationships indicated in the drawings for convenience in describing the present invention and to simplify the description, and are not intended to indicate or imply that the referenced devices or elements must be in a particular orientation, constructed and operated in a particular orientation, and are therefore not to be considered limiting of the present invention. The terms "first," "second," "third," and the like, herein do not denote any particular quantity or order, but rather are used to distinguish one element from another.
The structure of the sampling device used in the invention is shown in figure 1, and the sampling device comprises a support frame 1, wherein the support frame 1 comprises a working platform 11 and a support leg 12 vertically fixed at the bottom of the working platform 11; a vacuum cavity 2 is fixed on the support frame 1, one end of the vacuum cavity 2 is connected with a storage chamber 4 and a soil sample collection box 5 through a connecting assembly, the storage chamber 4 and the soil sample collection box 5 both have certain sealing performance, and the connection part of the storage chamber 4 and each pipeline can be connected by adopting a Ruhr joint; the other end of the vacuum cavity 2 is connected with a vacuum pump 6 through a vacuum pipeline. The connecting assembly comprises a first three-way joint 31, a second three-way joint 32 and a liquid suction head 33;
a first end of the first three-way joint 31 is connected with one end of the vacuum chamber 2 through a first pipeline 311; the second end of the first three-way joint 31 is connected with one end of the liquid suction head 33 through a second pipeline 312, and the other end of the liquid suction head 33 is placed in the soil sample collection box 5; the third end of the first three-way joint 31 is connected with the first end of the second three-way joint 32 through a third pipeline 313; the second end of the second three-way joint 32 is connected with the soil sample collection box 5 through a fourth pipeline 321; the third end of the second three-way joint 32 is connected with the storage chamber 4 through a fifth pipeline 322; the second pipeline 312 is provided with a first check valve 34, and the flow direction of the first check valve 34 is from bottom to top, that is, when liquid flows from bottom to top, the liquid can pass through the first check valve; when the liquid flows to the first one-way valve from top to bottom, the liquid is intercepted by the first one-way valve and cannot flow downwards continuously, the third pipeline 313 is provided with a second one-way valve 35, the flow direction of the second one-way valve 35 is opposite to that of the first one-way valve, and the second one-way valve is from top to bottom, namely the liquid can pass through the second one-way valve when flowing from top to bottom; when the liquid flows to the second one-way valve from bottom to top, the liquid is intercepted by the second one-way valve and cannot flow upwards continuously; a first electromagnetic valve 36 is installed on the fourth pipeline 321, and a second electromagnetic valve 37 is installed on the fifth pipeline 322;
soil sample gathers box 5 and is connected with agitator 7, the inside of soil sample gathering box 5 is stretched into to the agitator head of agitator 7. Further, the outside cladding of agitator 7 has silica gel cover 13, and silica gel cover 13 has certain cushioning effect, can avoid agitator 7 and soil sample collection box 5 direct contact through the outside cladding silica gel cover 13 at agitator 7, has certain guard action to soil sample collection box 5. Further, the stirring head of the stirrer 7 is a metal T-shaped stirring head.
The liquid suction head 33 is a polyester film liquid suction head, and a PVC thin tube is sleeved in the polyester film liquid suction head; one end of the polyester film liquid absorption head is sealed by an AB adhesive, and the other end of the polyester film liquid absorption head is connected with a second pipeline through a luer connector. Since the polyester film is too soft, in order to improve the flexibility, a PVC thin tube is sleeved inside the polyester film, so that a linear suction head is formed. When the liquid suction head is used, the liquid suction head made of the polyester film is bent and placed at the bottom of the soil sample collection box, the liquid level is guaranteed to be completely immersed, and the use efficiency of the liquid suction head is improved.
Further preferably, the support frame 1 is further provided with a control system 14 and a battery pack 15 for supplying power, and the control system 14 is electrically connected with the first electromagnetic valve 36, the second electromagnetic valve 37, the third electromagnetic valve 83, the fourth electromagnetic valve 84, the fifth electromagnetic valve 10 and the sixth electromagnetic valve 12; for the control system, a person skilled in the art can select an appropriate component composition according to specific needs; preferably, in the control system 14 of the present embodiment, the LCD1963 touch screen is used as an interactive interface, the STM32F103ZET6 single chip microcomputer is used as a core control unit, the voltage stabilizing chip LM1117 and the related load driving circuit MOS switch circuit are assisted, and the operation of the control system control device is controlled, so that the automation control can be realized, and the work efficiency is improved.
As another structural schematic diagram of the sampling device, referring to fig. 2, the vacuum pipeline includes a first vacuum pipeline 81 and a second vacuum pipeline 82, a third electromagnetic valve 83 is installed on the first vacuum pipeline 81, and a fourth electromagnetic valve 84 is installed on the second vacuum pipeline 82; one end of the first vacuum pipeline 81 is connected with the vacuum cavity 2, the other end of the first vacuum pipeline 81 is connected with the vacuum pump 6 through a third three-way joint 9, and a fifth electromagnetic valve 10 is installed at the free end of the third three-way joint 9; one end of the second vacuum pipeline 82 is connected with the vacuum cavity 2, the other end of the second vacuum pipeline 82 is connected with the vacuum pump 6 through a fourth three-way joint 11, and a sixth electromagnetic valve 12 is installed at the free end of the fourth three-way joint 11. Through dividing into first vacuum pipeline 81 and second vacuum pipeline 82 with the vacuum pipeline to set up corresponding solenoid valve, when the device was in the washing process, open corresponding solenoid valve, the washing liquid can directly be discharged from third three way connection, fourth three way connection's free end, improves cleaning efficiency.
The sampling of the soil solution was carried out using the sampling device shown in fig. 1, the operating method was as follows: firstly, cleaning a sampling device, wherein the cleaning steps are as follows: taking down the liquid suction head 33, and connecting the luer connector 16 on the cleaning pipeline; then, the vacuum chamber 2 is in a negative pressure state by adjusting the vacuum pump 6, under the action of the negative pressure in the vacuum chamber 2, the clean water in the cleaning pipeline sequentially passes through the first one-way valve 34, the second pipeline 312, the first three-way joint 31 and the first pipeline 311 to enter the vacuum chamber 2, and is kept for 2 min; the vacuum chamber 2 is in a positive pressure state by adjusting the vacuum pump 6, and the clean water in the vacuum chamber 2 flows down from the first pipeline 311, the third pipeline 313, the second one-way valve 35 and the second three-way joint 32 in sequence under the action of pressure and gravity, and finally flows into the soil sample collection box 5 and the storage chamber 4 through the fourth pipeline 321 and the fifth pipeline 322 respectively. In the flowing process of the clean water, the pipelines, the soil sample collecting box 5 and the storage chamber 4 can be respectively washed, and residual substances remained on the inner walls of the pipelines are taken away; repeating the above operations for three times, namely cleaning for three times;
after cleaning, connecting the luer connector 16 to a pipeline filled with an extracting agent, adjusting the vacuum pump 6 to enable the vacuum cavity 2 to be in a negative pressure state, sucking and temporarily storing the extracting agent in the vacuum cavity 2, and then switching the luer connector 16 to the liquid sucking head 33; in order to exhaust air in the liquid suction head 33 and improve the vacuum effect of the whole device, the liquid suction head 33 is completely soaked in an extracting agent before being connected into the luer connector 16; putting a soil sample collected on site into a soil sample collection box 5, closing a second electromagnetic valve 37, opening a first electromagnetic valve 36, then enabling the interior of a vacuum cavity 2 to be in a positive pressure state through a regulating vacuum pump 6, enabling an extracting agent located in the vacuum cavity 2 to flow down from a first pipeline 311, a third pipeline 313, a second one-way valve 35 and a second three-way joint 32 in sequence, entering the soil sample collection box 5 through the first electromagnetic valve 36, starting a stirrer 7, fully combining the soil sample and the extracting agent under the continuous stirring of the stirrer 7, and combining a heavy metal element in a soil mixed state and the extracting agent so as to be stripped; then the vacuum pump 6 is adjusted to enable the vacuum cavity 2 to be in a negative pressure state, and soil leaching liquor in the soil sample collection box 5 is sucked into the vacuum cavity 2 for temporary storage through the pressure difference 33; then, the first electromagnetic valve 36 is closed, the second electromagnetic valve 37 is opened, and the vacuum pump 6 is adjusted to make the interior of the vacuum chamber 2 in a positive pressure state, at this time, the soil leaching solution in the vacuum chamber 2 flows into the fifth pipeline 322 and then enters the storage chamber 4, and the soil leaching solution sampling operation is completed through the above steps.
After sampling is finished, the cleaning steps are repeated, the sampling device is cleaned, and then a new liquid suction head 33 is replaced to continue to be used for subsequent detection.
Examples
As an embodiment of the invention, the reagent used in the sampling method is the leaching agent A provided by the invention, and the preparation steps are as follows:
s1, preparing 0.02mol/L sodium hydroxide solution and 0.05mol/L borax solution, then taking 50ml of borax solution, gradually adding 0.02mol/L sodium hydroxide solution into the borax solution, measuring the pH value of the system once when 3ml of sodium hydroxide solution is added, and enabling the pH value of the mixed solution of borax and sodium hydroxide to be 9.5 to obtain alkaline buffer solution;
s2, adding 150g of sodium citrate crystals into 200ml of deionized water, performing vibration stirring by using an adjustable ultrasonic cleaner, wherein the power is 500w, the temperature is 50 ℃, the vibration stirring time is 10min until the sodium citrate crystals are not dissolved any more, so as to obtain a supersaturated mixed solution, taking out the supersaturated mixed solution, cooling the supersaturated mixed solution to room temperature for about 1h, performing centrifugal separation to remove solid substances, so as to obtain a saturated sodium citrate solution with the concentration of about 2.3mol/L at the room temperature, and naming the saturated sodium citrate solution as an extracting agent B;
s3, mixing 30g of Na2Adding EDTA powder into 200ml of leaching agent B, and stirring with an adjustable ultrasonic cleaner at a power of 700w and a temperature of 50 ℃ for 10min until Na is obtained2After EDTA powder is not dissolved any more, a supersaturated mixed solution is obtained, the mixture is taken out and cooled to room temperature for about 1 hour, and then Na saturated at room temperature is obtained after solid matters are removed by centrifugal separation2EDTA and sodium citrate mixed solution, named as leaching agent C;
s4, adding rhamnolipid into the extracting agent C, wherein the mass ratio of the rhamnolipid to the extracting agent C is 1:1000, and performing ultrasonic oscillation to obtain a solution, namely an extracting agent D;
s5, dropwise adding the alkaline buffer solution prepared in the step S1 into the leaching agent D, adjusting the pH value of the system to 9, and naming the obtained solution as leaching agent A.
Comparative example
For comparison, Na was prepared2The aqueous solution of EDTA is used as a contrast leaching agent, and the preparation method comprises the following steps: replacing the 200ml lixiviant B with 200ml deionized water in the step S3 of the previous embodiment, and keeping other operation conditions unchanged, thus obtaining Na2An aqueous solution of EDTA, designated lixiviant E.
The lixiviants prepared in the examples were subjected to soil treatment, the leaching rates of the lixiviants to metal ions were measured, and comparative experiments were conducted with lixiviant B, lixiviant C, lixiviant D, and lixiviant E. Wherein:
a leaching agent formula detection test is carried out according to the copper content in the Hebei moisture soil, the Hebei moisture soil is representative soil in the original region, and the basic physicochemical properties of the Hebei moisture soil are shown in the following table 1.
TABLE 1 basic physicochemical Properties of Hebei moisture soil
The test method for the leaching rate of Cu is: in the immersion test, the solid-to-liquid ratio of the soil sample to be detected to the leaching agent is kept at 1:8, the leaching time is 6 hours, the leaching solution is measured by using an atomic absorption plasma spectrometry, the leaching rate of Cu is statistically analyzed, and the results are shown in Table 2.
TABLE 2 mean value comparison of leaching rates of five leaching agents
| Kind of lixiviant | Lixiviant E | Lixiviant B | Lixiviant C | Lixiviant D | Lixiviant A |
| Leaching rate of Cu (%) | 36.7 | 27.27 | 42.90 | 43.75 | 46.48 |
As can be seen from Table 2, Na2EDTA and sodium citrate are excellent heavy metal leaching agents, and when used alone, can leach Cu in soil to a certain extent. When the two are used together, the synergistic effect can be achieved, and the leaching rate is improved. The extraction rate can be further improved by adding the surfactant rhamnolipid, and after the alkaline buffer solution is added, the extraction rate is greatly improved, because as the reaction proceeds, the alkalinity is weakened, the optimal extraction condition is destroyed, and the efficiency is reduced. In conclusion, when the two leaching agents are used in a supersaturated and mixed mode in an environment with an alkaline buffer solution, the leaching rate of the leaching agents can be optimized when the surfactant rhamnolipid is added.
Claims (10)
1. A sampling method for obtaining soil solution by high-efficiency online leaching is characterized by comprising the following steps: the method comprises the following steps:
adding borax into a sodium hydroxide solution to prepare an alkaline buffer solution; adding a chelating agent into a sodium citrate solution to obtain a mixed solution; adding a biosurfactant and an alkaline buffer solution into the mixed solution, and uniformly mixing to obtain an extractant;
and mixing the leaching agent with the soil sample to be detected, and separating heavy metal elements in the soil sample to be detected into the leaching agent through the soaking effect of the leaching agent on the soil to obtain a soil solution.
2. The sampling method according to claim 1, characterized in that: the pH value of the alkaline buffer solution is 9-10; the chelating agent is Na2One of EDTA, DTPA, DTPMA, EDTPMA and PBTCA; the biosurfactant is one of rhamnolipid, cellobiose and seaweed glycolipid.
3. The sampling method according to claim 2, characterized in that: the mass ratio of the biosurfactant to the mixed solution is 1: 1000.
4. The sampling method according to claim 1, characterized in that: the method for uniformly mixing is ultrasonic oscillation.
5. The sampling method according to claim 1, characterized in that: mixing an extracting agent and a soil sample to be detected in a sampling device, wherein the sampling device comprises a support frame, a vacuum cavity is fixed on the support frame, one end of the vacuum cavity is connected with a storage chamber and a soil sample collecting box through a connecting component, and the other end of the vacuum cavity is connected with a vacuum pump through a vacuum pipeline; the connecting assembly comprises a first three-way joint, a second three-way joint and a liquid suction head;
the first end of the first three-way joint is connected with one end of the vacuum cavity through a first pipeline; the second end of the first tee joint is connected with one end of a liquid suction head through a second pipeline, and the other end of the liquid suction head is placed in a soil sample collection box; the third end of the first three-way joint is connected with the first end of the second three-way joint through a third pipeline; the second end of the second three-way joint is connected with the soil sample collection box through a fourth pipeline; the third end of the second three-way joint is connected with the storage chamber through a fifth pipeline; a first one-way valve is arranged on the second pipeline, and a second one-way valve is arranged on the third pipeline; a first electromagnetic valve is installed on the fourth pipeline, and a second electromagnetic valve is installed on the fifth pipeline;
the soil sample collection box is connected with a stirrer, and a stirring head of the stirrer extends into the soil sample collection box.
6. The sampling method according to claim 5, wherein: the vacuum pipeline comprises a first vacuum pipeline and a second vacuum pipeline, a third electromagnetic valve is installed on the first vacuum pipeline, and a fourth electromagnetic valve is installed on the second vacuum pipeline; one end of the first vacuum pipeline is connected with the vacuum cavity, the other end of the first vacuum pipeline is connected with the vacuum pump through a third tee joint, and a fifth electromagnetic valve is installed at the free end of the third tee joint; one end of the second vacuum pipeline is connected with the vacuum cavity, the other end of the second vacuum pipeline is connected with the vacuum pump through a fourth three-way joint, and a sixth electromagnetic valve is installed at the free end of the fourth three-way joint.
7. The sampling method according to claim 5, wherein: a silica gel sleeve is coated outside the stirrer; the stirring head of the stirrer is a metal T-shaped stirring head.
8. The sampling method according to claim 5, wherein: the support frame is also provided with a battery pack for supplying power, and the battery pack is electrically connected with the first electromagnetic valve, the second electromagnetic valve, the third electromagnetic valve, the fourth electromagnetic valve, the fifth electromagnetic valve and the sixth electromagnetic valve.
9. The sampling method according to claim 5, wherein: the liquid absorption head is a polyester film liquid absorption head, and a PVC (polyvinyl chloride) thin tube is sleeved in the polyester film liquid absorption head; one end of the polyester film liquid absorption head is sealed by an AB adhesive, and the other end of the polyester film liquid absorption head is connected with a second pipeline through a luer connector.
10. A sampling method according to any one of claims 5 to 9, characterized in that: the support frame comprises a working platform and support legs vertically fixed at the bottom of the working platform.
Priority Applications (1)
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