CN110987726A - Method for in-situ monitoring two-dimensional plane migration of soil trace elements - Google Patents

Method for in-situ monitoring two-dimensional plane migration of soil trace elements Download PDF

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CN110987726A
CN110987726A CN201910891661.0A CN201910891661A CN110987726A CN 110987726 A CN110987726 A CN 110987726A CN 201910891661 A CN201910891661 A CN 201910891661A CN 110987726 A CN110987726 A CN 110987726A
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soil
membrane
trace elements
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film
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CN110987726B (en
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李志涛
张璠
赵玉杰
刘潇威
周其文
张闯闯
武鑫
王继军
孙杨
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Agro Environmental Protection Institute Ministry of Agriculture
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Abstract

The invention relates to a method for in-situ monitoring of two-dimensional planar migration of soil trace elements, which is a method for in-situ tracking and monitoring of trace element changes in flooded soil based on a gradient diffusion thin film (DGT) technology. The method realizes the activity change of the soil trace elements difficult to indicate in different depths of soil by conventional chemical extraction, and intuitively shows the migration rule of the soil elements due to factors such as oxidation-reduction reaction, substance migration and the like. The soil in-situ detection device is simple in structure and convenient to use, and can effectively evaluate the change of the soil trace elements.

Description

Method for in-situ monitoring two-dimensional plane migration of soil trace elements
Technical Field
The invention belongs to the field of soil trace element monitoring, and relates to a technology for realizing soil trace element in-situ monitoring by matching a simple pretreatment mode based on the DGT (differential gradients in the films) principle, in particular to a method for in-situ monitoring two-dimensional plane migration of soil trace elements.
Background
The soil-water interface is a common environmental interface in flooded soil environments such as paddy fields. Due to the existence of redox substances in soil, a severe redox gradient exists, so that the vertical migration distribution of soil trace elements is influenced. Conventional chemical extraction means such as one-step chemical extraction methods such as 0.01M calcium chloride, citric acid, 0.01M magnesium nitrate, 5mM DTPA, 3mM EDTA and the like, and multi-step chemical extraction methods such as BCR extraction and five-step extraction methods are difficult to indicate microscopic changes of soil trace elements in the interface, and elucidate the mechanism of activity change. At present, a precise detection instrument based on an Itrax device can carry out certain research on migration, migration and migration of soil trace elements and the like, but is expensive and high in cost. And in the process, destructive sampling methods are adopted, so that the soil disturbance is large.
In recent years, DGT technology (differential gradients in thinfilms) based on the principle of film gradient diffusion is widely applied to monitoring the active state of heavy metals in soil, water and sediments. DGT devices consist of a well-defined diffusion phase gel (diffusion membrane and filter) and a binding phase gel with strong complexing power. According to Fick's diffusion law, when the DGT device is in an ambient medium, the analyte to be detected passes through the filter membrane and the diffusion membrane gel, and is captured by the binding phase, thereby forming a stable linear concentration gradient at the diffusion layer. The combined phase material in the DGT technology can complex more than 30 elements such as Ca, Fe, Cu, Zn, Pb, Cd, Ni and the like in a complex natural environment, and can fully meet the requirement of synchronous monitoring of soil trace elements.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for in-situ tracking and monitoring the trace element change in flooded soil based on a gradient diffusion thin film (DGT) technology.
A method for in-situ monitoring two-dimensional plane migration of soil trace elements comprises the following steps:
(1) taking out the monitoring device from the self-sealing bag, washing residual solution on the surface of the device with ultrapure water, holding a handle of the device by hand, vertically inserting the device into a sample to be tested, wherein the humidity of the soil to be tested is required to reach 100% water content or a flooding environment, directly inserting the device into non-root test soil, reserving a hole by using the device before use if the test environment is a root zone or a native soil environment, and then inserting the device into the hole;
(2) taking out the monitoring device after 24 hours, properly moving the handle forward and backward along the vertical direction of the device, vertically extracting the device after soil is loosened, washing the soil on the surface of the device by using deionized water, using inclined water flow to prevent the surface of a window of the monitoring device from entering the device during washing, and wiping off redundant water on the surface by using absorbent paper;
(3) cutting along the window frame of the device by using a ceramic blade, removing the diffusion membrane on the surface by using a carbon fiber forceps, freezing for 5min at the temperature of-18 ℃ until the water on the surface of the combined membrane is condensed, taking out the combined membrane, cutting by using the ceramic blade according to the required size, and placing the cut combined membrane in a 10mL plastic test tube;
(4) elution monitorBinding film of the test device: 8mL of HNO pH 2 was added3And (3) eluting for 20min, uniformly mixing the eluent by using a vortex instrument, pouring the eluent out, and measuring the eluent by using AA/AFS/ICP-MS (acrylic acid/formaldehyde/inductively coupled plasma-Mass Spectrometry), wherein when the device is applied to soil with low effective state concentration or added with a high-efficiency soil conditioner, if the detection amount of elements to be measured in the eluent is lower than the detection limit of the instrument, the extraction time of the device can be adjusted to 2 days.
The monitoring device used in the method for in-situ monitoring of the two-dimensional plane migration of the trace elements in the soil comprises a jacket and an internal core assembly, wherein the jacket comprises a supporting plate and a sealing cover plate, the internal core assembly comprises a protective film, a diffusion film and a combination film, the sealing cover plate covers the supporting plate, a window is formed in the sealing cover plate, the protective film, the diffusion film and the combination film are packaged in the supporting plate and the sealing cover plate, the combination film, the diffusion film and the protective film are sequentially packaged from inside to outside, and the protective film is exposed outside the window.
Moreover, the supporting plate is made of a hard light-transmitting material of epoxy resin glass fiber board, namely FR-4 or acrylic.
Moreover, the sealing glue cover plate is a Chinese character 'hui' light-transmitting hard epoxy resin glass fiber plate or an acrylic plate.
Furthermore, the protective membrane is one of a nitrocellulose membrane with a pore size of 0.45 μm, a hydrophilic PVDF membrane, a polysulfone membrane or a dialysis membrane with an exclusion molecular weight of < 7000.
Furthermore, the diffusion membrane is an agarose gel or polyacrylamide gel membrane.
Furthermore, the choice of the binding membrane material is determined by the element to be detected.
When the target element is Fe2+、Cd2+、Cu2+、Ni2+、Co2+And Zn2+When the cation is generated, the binding phase material is DTPA modified Mg-Al-LDH; if the target element is S2-、PO4 3-、SeO4 2-Or SeO3 2-Anion, the binding phase material is Mg-Al-LDH; if Fe is co-extracted2+、Cd2+、Cu2+、Ni2+、Zn2+、Co2+、S2-、PO4 3-When the multi-element material is multi-element, the mass ratio of the binding phase material is 1: 1 Mg-Al-LDH and DTPA modified Mg-Al-LDH mixed material.
And the size of the outer frame of the support plate is 20 multiplied by 13cm, the thickness of the bottom plate is 2mm, an embedded groove which is 15cm long and 10cm wide is arranged at a position 1.5cm away from the bottom edge in an embedding manner, the depth of the groove is 1.53mm and is used for paving the diffusion film and the combination film, a glue sealing groove which is 0.5mm deep is additionally arranged outside the groove 5mm and is used for filling glue and adhering to a glue sealing cover piece, the thickness of the glue sealing cover piece is 1mm, the outer size of the glue sealing cover piece is 18cm multiplied by 13cm, and the inner size of the glue sealing cover piece is 14cm multiplied by.
Moreover, the monitoring device for in-situ monitoring the two-dimensional plane migration of the soil trace elements is manufactured by the following method: firstly, a layer of protective film is paved in a groove in a flat way, ultrapure water is sprayed to completely wet the protective film, a combination film and a diffusion film with the size of 15 multiplied by 10cm are paved on the protective film in sequence, a layer of nitrocellulose film protective film with the size of 16 multiplied by 11cm is paved on the outmost layer to cover a gallery around the groove so as to prevent soil seepage and water seepage, curable shadowless glue is filled in a glue sealing groove, a glue sealing cover piece provided with a window is aligned to a left frame, a right frame and a bottom frame, after the glue sealing cover piece is covered, an ultraviolet lamp is used for irradiating for more than 30 seconds to ensure the curing of the shadowless glue, the device is put into a sealing bag, and 5-8ml of 0.1mol/L sodium nitrate solution is added.
The invention has the advantages and positive effects that:
1. the device consists of a clearly defined diffusion phase gel (a diffusion membrane and a filter membrane) and a binding phase gel with strong complexing ability, according to Fick's diffusion law, when a DGT device is in an environmental medium, an analyte to be detected penetrates through the filter membrane and the diffusion membrane gel and is captured by a binding phase, so that a stable linear concentration gradient is formed in the diffusion layer, and a binding phase material in the DGT technology can complex more than 30 elements such as Ca, Fe, Cu, Zn, Pb, Cd, Ni and the like in a complex natural environment, so that the requirement on synchronous monitoring of trace elements in soil can be fully met.
2. The invention does not need the traditional conventional chemical extraction means such as one-step chemical extraction methods such as 0.01M calcium chloride, citric acid, 0.01M magnesium nitrate, 5mM DTPA, 3mM EDTA and the like, or multi-step chemical extraction methods such as BCR extraction and five-step extraction methods, is difficult to indicate the microscopic change of soil trace elements in the interface, and elucidates the mechanism of activity change, thereby being time-consuming, labor-consuming and expensive, and effectively protecting the inner layer membrane structure by the outer sleeve and the inner core component; the protective film is one of a nitrocellulose membrane, a hydrophilic PVDF membrane, a polysulfone membrane or a dialysis membrane with exclusion molecular weight less than 7000, the pore diameter of which is 0.45 mu m, so that impurities can be prevented from entering the diffusion membrane to influence the measurement result; the diffusion membrane is an agarose gel or polyacrylamide gel membrane, can promote the movement of metal ions, and has good adhesion effect; the combined membrane material has strong selectivity, and the size of the device is obtained through multiple tests, so that the in-situ monitoring of the soil trace elements is efficiently realized.
3. The invention provides a use method of a two-dimensional plane transfer device for in-situ monitoring of soil trace elements, which comprises the steps of cutting along a window frame by using a ceramic blade after detection is finished, removing a diffusion membrane on the surface by using a carbon fiber forceps, freezing for 5min at the temperature of-18 ℃, taking out after the surface of a combined membrane is condensed, cutting according to the required size by using the ceramic blade, placing the cut combined membrane in a 10mL plastic test tube, eluting the combined membrane, and carrying out efficient and rapid determination by using a formula.
4. The invention provides a device for in-situ monitoring of two-dimensional planar migration of soil trace elements and a using method thereof, the method is based on a gradient diffusion thin film (DGT) technology for in-situ tracking monitoring of trace element changes in flooded soil, the trace elements in the soil are detected by using a diffusion film and a combination film, different soil types are respectively calibrated, the detection method is standardized, a large amount of test operations are carried out, the in-situ detection of the trace elements in the soil under natural conditions is realized, the special scientific meaning for reflecting the oxidation-reduction condition of the soil under natural conditions is achieved, the technical problems that in-situ detection equipment in the prior art is expensive and inconvenient to carry, and the popularization and use of common laboratories are difficult are solved, the structure is simple, the use is convenient, and the changes of the trace elements in the soil are effectively evaluated.
Drawings
FIG. 1 is a front view of the apparatus of the present invention;
FIG. 2 is a side view (partially in section) of FIG. 1;
fig. 3 is a graph showing experimental results of migration changes of elements in soil on a two-dimensional plane in the embodiment of the invention.
Detailed Description
The present invention will be described in further detail with reference to the following embodiments, which are illustrative only and not limiting, and the scope of the present invention is not limited thereby.
A method for in-situ monitoring two-dimensional plane migration of soil trace elements comprises the following steps:
(5) taking out the monitoring device from the self-sealing bag, washing residual solution on the surface of the device with ultrapure water, holding a handle of the device by hand, vertically inserting the device into a sample to be tested, wherein the humidity of the soil to be tested is required to reach 100% water content or a flooding environment, directly inserting the device into non-root test soil, reserving a hole by using the device before use if the test environment is a root zone or a native soil environment, and then inserting the device into the hole;
(6) taking out the monitoring device after 24 hours, and in order to facilitate taking out of the device and reduce damage to the soil environment, properly moving the handle back and forth along the vertical direction of the device by hand, vertically extracting the device after soil is loosened, washing the soil on the surface of the device by deionized water, and wiping off excessive water on the surface by using absorbent paper when washing by using inclined water flow to prevent the window surface of the monitoring device from entering the device;
(7) cutting along the window frame of the device by using a ceramic blade, removing the diffusion membrane on the surface by using a carbon fiber forceps, freezing for 5min at the temperature of-18 ℃ until the water on the surface of the combined membrane is condensed, taking out the combined membrane, cutting by using the ceramic blade according to the required size, and placing the cut combined membrane in a 10mL plastic test tube;
(8) elution of binding membrane of monitoring device: 8mL of HNO pH 2 was added3Eluting for 20min, mixing with a vortex instrument, pouring out eluate, and measuring with AA/AFS/ICP-MS when the concentration of the device is low or high-efficiency soil conditioner is addedWhen the device is applied to the soil, if the detection amount of elements to be detected in the eluent is lower than the detection limit of the instrument, the extraction time of the device can be adjusted to 2 days.
The monitoring device used in the method for in-situ monitoring of the two-dimensional plane migration of the trace elements in the soil comprises a jacket and an internal core component, wherein the jacket is composed of a support plate 1 and a sealing cover sheet 2, the internal core component is composed of a protective film 4, a diffusion film 6 and a bonding film 5, the sealing cover sheet covers the support plate, the support plate is made of an epoxy resin glass fiber board, namely FR-4, or one of acrylic hard light-transmitting materials, the sealing cover sheet is a light-transmitting hard epoxy resin glass fiber board shaped like a Chinese character 'hui' or an acrylic board, a window 3 is formed in the sealing cover sheet, the protective film, the diffusion film and the bonding film are packaged in the support plate and the sealing cover sheet, the bonding film, the diffusion film and the protective film are sequentially packaged from inside to outside, and the protective film is exposed outside the window.
The protective membrane is one of a nitrocellulose membrane, a hydrophilic PVDF membrane, a polysulfone membrane or a dialysis membrane with exclusion molecular weight less than 7000, the pore diameter of the protective membrane is 0.45 mu m, the diffusion membrane is an agarose gel or polyacrylamide gel membrane, and the selection of the combined membrane material is determined by elements to be detected: when the target element is Fe2+、Cd2+、Cu2+、Ni2+、Co2+And Zn2+When the cation is generated, the binding phase material is DTPA modified Mg-Al-LDH; if the target element is S2-、PO4 3-、SeO4 2-Or SeO3 2-Anion, the binding phase material is Mg-Al-LDH; if Fe is co-extracted2+、Cd2+、Cu2+、Ni2+、Zn2+、Co2+、S2-、PO4 3-When the multi-element material is multi-element, the mass ratio of the binding phase material is 1: 1 Mg-Al-LDH and DTPA modified Mg-Al-LDH mixed material.
The size of the outer frame of the supporting plate is 20 multiplied by 13cm, the thickness of the bottom plate is 2mm, an embedded groove which is 15cm long and 10cm wide is embedded at a position 1.5cm away from the bottom edge, the depth of the embedded groove is 1.53mm and is used for paving a diffusion film and a combination film, a glue sealing groove which is 0.5mm deep is additionally arranged outside the groove 5mm and is used for filling glue and adhering a glue sealing cover piece, the thickness of the glue sealing cover piece is 1mm, the outer size of the glue sealing cover piece is 18cm multiplied by 13cm, and the inner size of the glue sealing cover piece is 14cm multiplied by 9 cm.
The monitoring device for in-situ monitoring of the two-dimensional plane migration of the soil trace elements is manufactured by the following steps: firstly, a layer of protective film is paved in a groove in a flat way, ultrapure water is sprayed to completely wet the protective film, a combination film and a diffusion film with the size of 15 multiplied by 10cm are paved on the protective film in sequence, a layer of nitrocellulose film protective film with the size of 16 multiplied by 11cm is paved on the outmost layer to cover a gallery around the groove so as to prevent soil seepage and water seepage, curable shadowless glue is filled in a glue sealing groove, a glue sealing cover piece provided with a window is aligned to a left frame, a right frame and a bottom frame, after the glue sealing cover piece is covered, an ultraviolet lamp is used for irradiating for more than 30 seconds to ensure the curing of the shadowless glue, the device is put into a sealing bag, and 5-8ml of 0.1mol/L sodium nitrate solution is added.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The soil sample for the research is collected from rice soil in Mianzhu city, Sichuan province, the soil is uniformly taken from a plough layer (0-20cm), and 7kg of the soil is taken and ground through a 2mm sieve after being naturally dried, and is stored for later use. The root system box is placed in a root system box with a root system grid with the width of 3 centimeters, and the size of the root system box is 20 multiplied by 20 cm. Submerging and maintaining the water depth of the liquid surface to be about 2cm, and planting rice after the soil is stabilized for 15 days. And extracting soil elements such as S, Ca, Fe, Mn, Cu, Zn, Cd and the like from root-system soil and non-root-system soil by using flat equipment in a seedling stage, a tillering stage, a flowering stage and a grouting stage respectively. The operation method and process of the device are as described above, and the change of the two-dimensional plane is reflected according to the monitored value of the eluent, and the result is shown in fig. 3.
Although the embodiments of the present invention and the accompanying drawings are disclosed for illustrative purposes, those skilled in the art will appreciate that: various substitutions, changes and modifications are possible without departing from the spirit and scope of the invention and the appended claims, and therefore the scope of the invention is not limited to the disclosure of the embodiments and the accompanying drawings.

Claims (10)

1. A method for in-situ monitoring two-dimensional plane migration of soil trace elements is characterized by comprising the following steps: the method comprises the following steps:
(1) taking out the monitoring device from the self-sealing bag, washing residual solution on the surface of the device with ultrapure water, holding a handle of the device by hand, vertically inserting the device into a sample to be tested, wherein the humidity of the soil to be tested is required to reach 100% water content or a flooding environment, directly inserting the device into non-root test soil, reserving a hole by using the device before use if the test environment is a root zone or a native soil environment, and then inserting the device into the hole;
(2) taking out the monitoring device after 24 hours, properly moving the handle forward and backward along the vertical direction of the device, vertically extracting the device after soil is loosened, washing the soil on the surface of the device by using deionized water, using inclined water flow to prevent the surface of a window of the monitoring device from entering the device during washing, and wiping off redundant water on the surface by using absorbent paper;
(3) cutting along the window frame of the device by using a ceramic blade, removing the diffusion membrane on the surface by using a carbon fiber forceps, freezing for 5min at the temperature of-18 ℃ until the water on the surface of the combined membrane is condensed, taking out the combined membrane, cutting by using the ceramic blade according to the required size, and placing the cut combined membrane in a 10mL plastic test tube;
(4) elution of binding membrane of monitoring device: 8mL of HNO pH 2 was added3And (3) eluting for 20min, uniformly mixing the eluent by using a vortex instrument, pouring the eluent out, and measuring the eluent by using AA/AFS/ICP-MS (acrylic acid/formaldehyde/inductively coupled plasma-Mass Spectrometry), wherein when the device is applied to soil with low effective state concentration or added with a high-efficiency soil conditioner, if the detection amount of elements to be measured in the eluent is lower than the detection limit of the instrument, the extraction time of the device can be adjusted to 2 days.
2. The method for in-situ monitoring of two-dimensional planar migration of trace elements in soil according to claim 1, wherein: the monitoring device used in the method for in-situ monitoring of the two-dimensional plane migration of the soil trace elements comprises a jacket and an internal core assembly, wherein the jacket consists of a supporting plate and a sealing cover plate, the internal core assembly consists of a protective film, a diffusion film and a combination film, the sealing cover plate covers the supporting plate, a window is formed in the sealing cover plate, the protective film, the diffusion film and the combination film are packaged in the supporting plate and the sealing cover plate, the combination film, the diffusion film and the protective film are sequentially packaged from inside to outside, and the protective film is exposed outside the window.
3. The method for in-situ monitoring of two-dimensional planar migration of trace elements in soil according to claim 2, wherein: the supporting plate is made of an epoxy resin glass fiber board, namely FR-4 or acrylic hard light-transmitting material.
4. The method for in-situ monitoring of two-dimensional planar migration of trace elements in soil according to claim 2, wherein: the sealing glue cover plate is a light-transmitting hard epoxy resin glass fiber plate or an acrylic plate in a shape like a Chinese character 'hui'.
5. The method for in-situ monitoring of two-dimensional planar migration of trace elements in soil according to claim 2, wherein: the protective membrane is one of a nitrocellulose membrane with the pore diameter of 0.45 mu m, a hydrophilic PVDF membrane, a polysulfone membrane or a dialysis membrane with the exclusion molecular weight less than 7000.
6. The method for in-situ monitoring of two-dimensional planar migration of trace elements in soil according to claim 2, wherein: the diffusion membrane is an agarose gel or polyacrylamide gel membrane.
7. The method for in-situ monitoring of two-dimensional planar migration of trace elements in soil according to claim 2, wherein: the choice of binding membrane material is determined by the element to be detected.
8. The method for in-situ monitoring of two-dimensional planar migration of trace elements in soil according to claim 7, wherein: when the target element is Fe2+、Cd2+、Cu2+、Ni2+、Co2+And Zn2+When the cation is generated, the binding phase material is DTPA modified Mg-Al-LDH; if the target element is S2-、PO4 3-、SeO4 2-Or SeO3 2-Anion, the binding phase material is Mg-Al-LDH; if Fe is co-extracted2+、Cd2+、Cu2+、Ni2+、Zn2+、Co2+、S2-、PO4 3-When the multi-element material is multi-element, the mass ratio of the binding phase material is 1: 1 Mg-Al-LDH and DTPA modified Mg-Al-LDH mixed material.
9. The method for in-situ monitoring of two-dimensional planar migration of trace elements in soil according to claim 2, wherein: the size of the outer frame of the supporting plate is 20 multiplied by 13cm, the thickness of the bottom plate is 2mm, an embedded groove which is 15cm long and 10cm wide is embedded at a position 1.5cm away from the bottom edge, the depth of the embedded groove is 1.53mm and is used for paving a diffusion film and a combination film, a glue sealing groove which is 0.5mm deep is additionally arranged outside the groove 5mm and is used for filling glue and adhering a glue sealing cover piece, the thickness of the glue sealing cover piece is 1mm, the outer size of the glue sealing cover piece is 18cm multiplied by 13cm, and the inner size of the glue sealing cover piece is 14cm multiplied by 9 cm.
10. The method for in-situ monitoring of two-dimensional planar migration of trace elements in soil according to claim 2, wherein: the monitoring device for in-situ monitoring the two-dimensional plane migration of the soil trace elements is manufactured by the following steps: firstly, a layer of protective film is paved in a groove in a flat way, ultrapure water is sprayed to completely wet the protective film, a combination film and a diffusion film with the size of 15 multiplied by 10cm are paved on the protective film in sequence, a layer of nitrocellulose film protective film with the size of 16 multiplied by 11cm is paved on the outmost layer to cover a gallery around the groove so as to prevent soil seepage and water seepage, curable shadowless glue is filled in a glue sealing groove, a glue sealing cover piece provided with a window is aligned to a left frame, a right frame and a bottom frame, after the glue sealing cover piece is covered, an ultraviolet lamp is used for irradiating for more than 30 seconds to ensure the curing of the shadowless glue, the device is put into a sealing bag, and 5-8ml of 0.1mol/L sodium nitrate solution is added.
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