CN113769717A - Preparation method and application of adsorption film in DGT device - Google Patents
Preparation method and application of adsorption film in DGT device Download PDFInfo
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Abstract
The invention discloses a preparation method and application of an adsorption film in a DGT device, and belongs to the field of environmental chemistry. The adsorption membrane adopts agarose gel as hydrogel, the adsorption material is directly synthesized in the hydrogel, the hydrogel prepared by the method still keeps transparent, and no wrinkle is generated when the adsorption material is zirconium oxide. The adsorption film overcomes the problems that the existing adsorption film for detecting oxoanion has long preparation period, water absorption expansion and wrinkles to influence flat scanning, has good detection effect and can be produced on a large scale.
Description
Technical Field
The invention belongs to the field of environmental chemistry, and particularly relates to a preparation method and application of an adsorption film in a DGT (defected ground test) device.
Background
The gradient diffusion membrane technology (DGT) was invented in 1994 by William Davison and Hao Zhang, university of Lancassetti, England, and its principle is that the element to be measured is irreversibly adsorbed by the adsorption membrane (Resin gel) after passing through the diffusion membrane (Diffusive gel). Because the flux (or diffusion coefficient) is only related to the environmental concentration and temperature of the object to be detected, the environmental concentration can be obtained by the Fick first law formula after the absorption capacity on the absorption film is obtained by instrument analysis. As an in-situ non-destructive passive sampling technique, the DGT technique is widely applied to the determination of metal cations and oxygen-containing anions in effective states in water, soil and sediments.
DGT devices consist of a stack of a fixed layer (i.e., an adsorbent film) and a diffusion layer (i.e., a diffusion film), the adsorbent film typically being made of an adsorbent material embedded in a gel, the determination of which depends on the type of adsorbent material. In the prior art, the preparation of adsorption membranes for detecting oxidizing anions in DGT is mainly Based on Guan Dongxing et al (Guin et al, Novel detected Zirconia-Based DGT technique for High-Resolution Imaging of Oxyanion in Waters and derivatives, Envir.&Technol.2015(49)3653-3661), which specifically comprises the following steps: (1) preparing polyacrylamide hydrogel (Luo, J.; Zhang, H.; Santner, J.; Davison, W.Performance Characteristics of differential gradients in which films are used to regulate with a binding gel layer containing sensitive polymeric (V), selected (VI), variable (V), and antibiotic (V), anal. chem.2010,82 (21)), 8903-8909.; (2) soaking the formed polyacrylamide hydrogel in 1mol L-1ZrOCl2At least 2 hours in solution; (3) after the surface of the soaked polyacrylamide gel is quickly washed, the polyacrylamide gel is soaked in 0.05mol L-1Rapidly oscillating in 2-morpholine ethanesulfonic acid (MES) solution with pH value of 6.7-6.8 for 40 min; (4) and (4) performing replacement washing in the deionized water for a plurality of times (each time of soaking for at least 1 hour) until the pH value of the deionized water solution after replacement is about 5.6 +/-0.3. The above method has the following disadvantages: (1) firstly, preparing, cleaning and preparing the polyacrylamide hydrogel, and the time consumption is as long as 3 days; (2) since the acrylamide gel swells by absorbing water after polymerization, it must be first formed into a sheetThe hydrogel is sliced and assembled after being expanded, so that the absorption film cannot be directly formed on a product part at one time, the volume is kept unchanged, and the mass production is not facilitated; (3) after zirconium oxide is precipitated on acrylamide gel, hydrogel becomes very hard, and the hydrogel needs to oscillate during precipitation, so that the hydrogel has many folds (as shown in fig. 4), the folds cannot be smoothed, when the adsorption capacity is measured by combining a computer density imaging metering (CID) technology, if direct scanning seriously affects data accuracy, spatial displacement of unpredictable and corrective data points, flat scanning is not suitable for direct color development, and the detection efficiency is reduced.
Disclosure of Invention
1. Problems to be solved
The invention develops a preparation method and application of a novel agarose gel adsorption membrane, aiming at the problems of long preparation period, water swelling, fold influence on flat scanning and the like of the adsorption membrane used in the technology for detecting the DGT of the oxyanion.
2. Technical scheme
In order to solve the problems, the technical scheme adopted by the invention is as follows:
the invention provides an adsorption film in a DGT device, which comprises an adsorption material and hydrogel, wherein the hydrogel is agarose gel.
Preferably, the adsorbent is an adsorbent such as Zr-oxide or Ti-oxide.
The invention provides a preparation method of an adsorption film in a DGT device, which comprises the following steps:
(1) dissolving: ZrOCl2·8H2Dissolving O and agarose powder in water;
(2) heating: heating the mixed solution in the step (1) until the solution becomes clear;
(3) and (3) cooling: injecting the heated mixed solution into a corresponding mould for cooling;
(4) and (3) precipitation: soaking the cooled hydrogel in 2- (N-morpholine) ethanesulfonic acid (MES) buffer solution and oscillating;
(5) washing: and (4) replacing and washing the soaked hydrogel with deionized water.
Preferably, in step (1), the water is deionized water.
Preferably, in step (1), ZrOCl is added relative to 100mL of deionized water2·8H2The dosage of O is 2-4g, and the dosage of agarose powder is 1-2 g. Further, ZrOCl2·8H2The amount of O was 3.22g and the amount of agarose powder was 1.5 g.
Preferably, in the step (2), the mixed solution is heated to 70 to 90 ℃. Further, the mixed solution was heated to 80 ℃.
Preferably, in step (2), the heating is carried out in a cold water bath.
Preferably, in the step (3), the cooling temperature is 4 ℃ or natural cooling.
Preferably, in step (4), the pH of the MES solution is from 6.7 to 6.8.
Preferably, in the step (4), the soaking time is 1 to 3 hours, and further, the soaking time is 2 hours.
Preferably, in step (5), the rinsing comprises soaking the hydrogel in deionized water for at least 0.5 to 1.5 hours, and further, for at least 1 hour.
Preferably, in the step (5), the deionized water is used for rinsing until the pH value of the deionized water solution after rinsing is 5.6 +/-0.3.
The invention also provides the adsorption film prepared by the preparation method.
The invention also provides the application of the adsorption film and the preparation method of the adsorption film in a DGT device.
Preferably, the application of the adsorption film and the adsorption film preparation method in the DGT device comprises a DGT device which comprises a diffusion film and an adsorption film, wherein the adsorption film is the adsorption film or the adsorption film prepared by the preparation method, and the DGT device can be used for detecting oxidized anions in water, sediment, soil and the like.
Preferably, the DGT device further comprises a filter.
The invention also provides the application of the DGT device in detecting the oxide anions in water, sediment, soil and the like.
Preferably, the invention also provides the application of the DGT device in phosphorus content determination.
The invention also provides a using method of the DGT device, which comprises the following steps:
(1) putting in the device: the device is put in an environmental medium (such as water, soil or sediment), enriched for a certain time and recorded with temperature;
(2) recovering the device: taking the DGT device out of the environment medium, and thoroughly cleaning the surface of the device by using deionized water;
(3) the device develops color: putting the device or the adsorption film into a color developing agent for color development;
(4) analysis and data processing: after the color development is completed, the data is analyzed and processed.
Preferably, the preparation method of the color developer in the step (3) comprises the following steps:
(a) preparing a solution A: an ammonium molybdate solution;
(b) preparing a solution B: antimony potassium tartrate solution;
(c) preparing a solution C: fully mixing the solution A and the solution B with a sulfuric acid solution;
(d) preparing a color developing agent: the ascorbic acid solution was mixed with solution C.
Preferably, in step (a), the amount of ammonium molybdate used is 8 to 32g relative to 100mL of deionized water. Further, the amount is 16 g.
Preferably, in step (b), the amount of antimony potassium tartrate used is 0.14 to 0.42g relative to 100mL of deionized water. Further, the amount is 0.28 g.
Preferably, in step (c), the amount of solution A is 3mL and the amount of solution B is 1mL relative to 10mL of 2.5M sulfuric acid solution;
preferably, in the step (d), 1.76g of ascorbic acid is fully dissolved in 100mL of deionized water, 6mL of the solution is mixed with 14mL of solution C, and then the mixture is diluted to 100mL by using the deionized water to form the final color developing agent, wherein the color developing agent contains 0.0226M MoO4 2-And 8.6mM Vc-The pH is stabilized at 0.5 +/-0.02.
Preferably, in the step (3), the device is placed into a color developing agent for color development, the liquid level of the color developing agent is 5mm above the sampling window of the DGT device, and the color development time is 15-30 min. Furthermore, the liquid surface of the color developing agent is 5mm higher than the sampling window of the DGT device, and the color developing time is 20 minutes.
Preferably, the analysis and data processing in step (4) can be performed by methods conventional in the art, or can be performed in combination with CID technology.
Preferably, the above-mentioned binding CID technique comprises the steps of:
(1) shaking the surface of the washing device;
(2) taking out the adsorption film or placing the adsorption film or the device on an office or household flat-panel scanner to scan and store the color development surface; or when the sample amount is small, scanning and storing by using a handheld color difference meter;
(3) the color was converted to gray using ImageJ software and quantitative calculations were performed using a standard curve.
Preferably, in the step (1), pouring out the color developing agent in the color developing tank, replacing deionized water, and shaking the surface of the washing device once (5 seconds);
preferably, the scanner resolution is set to 100 and 200dpi in step (2), and further, the scanner resolution is set to 150 dpi.
Preferably, the standard curve in step (3) is y ═ -104.3821e-0.3278x+118.7856 wherein x is per cm2Average gray scale of (1), y is per cm2The accumulated amount of phosphorus in (1).
3. Advantageous effects
Compared with the prior art, the invention has the beneficial effects that:
(1) compared with the adsorption film in the prior art, the adsorption film is completely transparent, and the active elements adsorbed on the adsorption film can be quantitatively analyzed from the front side and the back side by a color development method.
(2) According to the preparation method of the adsorption membrane, agarose gel is adopted, compared with the prior art, the polyacrylamide gel used for conventional DGT is very soft and elastic, and in the process of Zr-oxide precipitation, the gel can be inevitably bent or folded due to continuous oscillation, and when Zr-oxide is directly precipitated on the gel, the gel can be gradually hardened along with the reaction, so that the Zr-oxide gel formed by precipitation is not in a horizontal stretching state but has a plurality of fluctuated folds in a natural state under the condition of not applying a large external force; the agarose hydrogel is brittle and hard, has small elasticity, does not generate bending wrinkles in the oscillation process, has no obvious difference in the appearance shape of the gel before and after the Zr-oxide precipitation is finished, does not form wrinkles on the gel, is convenient for flat scanning, can be directly analyzed when being combined with a computer density imaging measurement (CID) technology to measure the adsorption quantity, and does not influence the detection accuracy. However, the adsorption film in the prior art has many wrinkles, which cannot be used for flat scanning analysis, and these wrinkles cannot be smoothed, and when the adsorption amount is measured by combining a computer density imaging measurement (CID) technology, if direct scanning would seriously affect the data accuracy, unpredictable data points and the corrected spatial displacement, the adsorption film is not suitable for flat scanning after direct color development, so that the detection efficiency is reduced.
(3) The preparation method of the adsorption film avoids the time-consuming process of preparing, cleaning and modulating the polyacrylamide hydrogel in advance, saves the time for 2 days, and has higher preparation efficiency.
(4) The preparation method of the adsorption membrane of the invention has the advantages that the formed agarose gel prepared by the method can not absorb water to expand, is beneficial to being directly poured into product parts and mass production, and avoids the process that the polyacrylamide hydrogel is firstly made into sheet hydrogel and then is cut into pieces to be assembled after being expanded.
Drawings
FIG. 1 is a diagram of a transparent Zr-oxide adsorption film based on agarose gel;
FIG. 2 is a diagram of a DGT apparatus based on a transparent Zr-oxide adsorption film;
FIG. 3 is a graph of the results obtained after sampling a long plate type DGT device in the lake Tai sediment;
FIG. 4 is a diagram of a conventional polyacrylamide-based Zr-oxide hydrogel;
FIG. 5 is a gray scale graph of a DGT device based on a transparent Zr-oxide adsorption film after adsorbing different amounts of phosphorus and developing color;
FIG. 6 is a gray scale plot of a DGT device after adsorbing varying amounts of phosphorus and developing color based on a conventional Zr-oxide adsorption film;
FIG. 7 shows the measurement of KH in aqueous solution by the apparatus of the present invention and a conventional DGT apparatus at different pH values2PO4The content of (A);
FIG. 8 shows the measurement of KH in aqueous solution by the device of the present invention and a conventional DGT device under different ionic strengths2PO4The content of (a).
Detailed Description
The invention is further described with reference to specific examples.
It is to be noted that the terms used in the present invention have meanings commonly understood by those skilled in the art unless otherwise specified. The invention is described in further detail below with reference to specific embodiments and with reference to the attached drawings. It should be noted that these examples are only intended to illustrate the present invention, and do not limit the scope of the present invention in any way.
Example 1
The embodiment provides a preparation method of an adsorption film, which comprises the following steps:
(1) 3.22g of ZrOCl were weighed into a beaker2·8H2O, 1.5g of agarose powder (Bio-rad), 100mL of deionized water were added;
(2) heating the mixed solution in the step (1) to 80 ℃ in a cold water bath until the solution becomes clear;
(3) injecting the heated mixed solution into a corresponding mould, and naturally cooling or cooling in a refrigerator at 4 ℃;
(4) soaking the cooled hydrogel in MES solution with pH of 6.7-6.8 for 2 hr;
(5) and (4) performing replacement washing in the deionized water for a plurality of times (each time of soaking for at least 1 hour) until the pH value of the deionized water solution after replacement is about 5.6 +/-0.3.
As shown in FIG. 1, the adsorption film prepared by the present invention is transparent and wrinkle-free, and facilitates flat-panel scanning.
Example 2
This example provides a DGT device with no wrinkle adsorption membrane, as shown in FIG. 2, comprising a filter membrane, a diffusion membrane, an adsorption membrane and a housing, where the adsorption membrane is the transparent adsorption membrane prepared in example 1, and the device can be used for measuring the phosphorus content in soil and sediment. The application of the device in measuring the phosphorus content in the lake Tai sediment specifically comprises the following steps:
(1) sampling, vertically burying a long plate type DGT device in the sediment, and standing for 24 hours;
(2) developing color, taking out the adsorption film in the DGT device, and dyeing, wherein the preparation of the color developing agent comprises the following steps: fully dissolving 16g of ammonium molybdate into 100mL of deionized water to prepare a solution A; fully dissolving 0.28g of antimony potassium tartrate into 100mL of deionized water to prepare a solution B; fully mixing 3mL of solution A and 1mL of solution B with 10mL of 2.5M sulfuric acid solution to prepare solution C; fully dissolving 1.76g of ascorbic acid into 100mL of deionized water, mixing 6mL of the solution with 14mL of solution C, and diluting with deionized water to 100mL to form the final color developing agent, wherein the color developing agent contains 0.0226M MoO4 2-And 8.6mM Vc-The pH value is stabilized at 0.5 +/-0.02; the results are shown in FIG. 3;
(3) and (3) detecting, namely calculating the content of phosphorus in the sediment and longitudinal two-dimensional high-resolution distribution by using the scanning gray of a flat plate.
Example 3
This example compares the color development uniformity of a DGT device comprising an adsorption film of the invention with that of a conventional DGT device. The specific method comprises the following steps:
experiment on 7 groups of 2L 0.01mol/L NaNO3The reaction is carried out in a solution (Analar, VWR), wherein the solution contains 20 to 2000. mu.g/L of monopotassium phosphate (Analar, VWR), and the solution is mixed for 12 hours by a magnetic stirrer, so that carbon dioxide in the air and the solution reach an equilibrium state. After stirring for 12 hours, the DGT apparatus was placed in the solution to enrich the orthophosphate in the solution for 4 hours. Meanwhile, 3 DGT devices are packaged by food-grade clean plastic bags for blank value measurement, and the DGT devices are processed by the same method as other DGT devices at the end of the experiment.
The results are shown in Table 1 and FIGS. 5 to 6, and the conventional Zr-oxide DGT device and the transparent Zr-oxide DGT device of the present application can be used for the detection of P, and the difference between the color development uniformity of the detection results is as follows:
the variation coefficient (standard deviation/average gray scale) of the novel transparent Zr-oxide DGT device is smaller than that of the conventional DGT device, and the variation coefficient and the standard deviation/average gray scale are very obvious different (P is less than 0.005), so that the novel device is obviously superior to the conventional product in color development uniformity.
Table 1: comparison of standard deviation and variation coefficient of conventional Zr-oxide DGT device and transparent Zr-oxide DGT device under different P enrichment
Example 4
This example provides the use of the adsorption film of the invention in a transparent DGT device.
The embodiment provides a transparent DGT device, which comprises an outer shell, an inner shell, a transparent adsorption film, a diffusion film, a filter film and a waterproof label, wherein the outer shell is a hollow structure; the adsorption film, the diffusion film and the filter film are sequentially placed in the inner shell from bottom to top; the inner shell is embedded in the outer shell, the outer shell is parallel to the bottom of the inner shell, and the top of the outer shell is higher than the inner shell and extends inwards for a certain length; the waterproof label covers the bottom of the inner shell and the outer shell. In the device, an inner shell is embedded in an outer shell, the inner diameter of the inner shell is 30mm, the height of the inner shell is 1.3mm, the bottom thickness (A surface) of the inner shell is 1mm, the thickness of a vertical wall (B surface) of the inner shell is 2mm, and the outer surface of the vertical wall (and the outer shell) is frosted and can be made of transparent and high-hardness materials such as PMMA (polymethyl methacrylate), glass-like PC (polycarbonate) or glass; the inner diameter of the outer shell is 34mm, the height is 2.3mm, the thickness is 2mm, the diameter of a sampling window (the surface in direct contact with the filter membrane) is 25mm, and the outer shell can be made of ABS material and has frosted appearance; the bottom is waterproof label, plays the effect of mark DGT device, protection transparent scanning face (A face), tears before the color development.
This example provides the apparatus of the present invention and a conventional DGT apparatus for measuring KH in aqueous solution2PO4The content comparison comprises the following steps:
(1) sampling
6 of the present example (new) transparent DGT devices and 6 of the conventional (conventional) DGT devices (the adsorption film was an iron oxide film,www.dgtresearch.comproduct number LSNP-NP on website) is placed in the place containing KH2PO4In the solution of (1);
the solution was prepared as follows: (a) 4mL of the solution was added to a reactor, and the solution was stirred at 100mg L-1KH of phosphorus2PO4The solution was added to 2L of deionized water to make 200. mu. g L-1The solution of (1); (b) by adding different quality NaNO into the solution3To adjust the ionic strength of the solution; (c) by adding different volumes of NaOH (1M) and HNO to this solution3(1M) to adjust the pH of the solution; (d) the solution needs to be continuously stirred in an open system (magnetic stirrer, 400-2A dynamic equilibrium state is reached; (5) the time of the experiment (not less than 4 hours) and the average water temperature during the experiment were recorded.
(2) Color development
Taking out the DGT device, and dyeing:
(a) novel DGT device dyeing method
Putting the DGT device into a color developing agent for color development, wherein the liquid surface of the color developing agent is 5mm higher than a sampling window of the DGT device, and the color developing time is 20 minutes; the preparation of the color developing agent comprises the following steps:
fully dissolving 16g of ammonium molybdate into 100mL of deionized water to prepare a solution A; fully dissolving 0.28g of antimony potassium tartrate into 100mL of deionized water to prepare a solution B; fully mixing 3mL of solution A and 1mL of solution B with 10mL of 2.5M sulfuric acid solution to prepare solution C; fully dissolving 1.76g of ascorbic acid into 100mL of deionized water, mixing 6mL of the solution with 14mL of solution C, and diluting with deionized water to 100mL to form the final color developing agent, wherein the color developing agent contains 0.0226M MoO4 2-And 8.6mM Vc-The pH is stabilized at 0.5 +/-0.02.
(b) Conventional DGT (LSNP-NP) is developed according to the standard method described in the following websitehttps:// www.dgtresearch.com/wp-content/uploads/2020/11/Phosphate-FeO-LSNP-26-10- 20.pdf。
(3) Detection of
The concentration of phosphorus in the experimental solution was calculated using the plate scan gray scale. The conventional DGT is calculated according to the enrichment obtained by the method of the website.
As shown in FIGS. 7 and 8, the monitoring results of the novel DGT and the driving DGT are not significantly different, and both can accurately predict the concentration of P in the experimental solution and the concentration of the solution directly obtained by the EPA365.2 standard method (C)S) Ratio (C) ofDGT/CS) Are all between 0.9 and 1.1, and have standard deviations within 7%.
The DGT device of this embodiment, adsorption film and nexine shell bottom are transparent, after adsorbing active element and dyeing, can be under the condition that does not take out the adsorption film, accomplish the effective scanning that can the quantitative computation adsorption capacity from DGT device nexine shell bottom, owing to need not disassemble the DGT device one by one, the DGT device can be a large amount of soak simultaneously in the colour-developing agent, and large-scale sample analysis, make sample treatment and analysis efficiency show the improvement, the device, the sampling, the analysis cost can effectively reduce.
Claims (10)
1. A method for preparing an adsorption film in a DGT device is characterized by comprising the following steps:
(1) dissolving: ZrOCl2·8H2Dissolving O and agarose powder in water;
(2) heating: heating the mixed solution in the step (1) until the solution becomes clear;
(3) and (3) cooling: injecting the heated mixed solution into a corresponding mould for cooling;
(4) and (3) precipitation: soaking the cooled hydrogel in MES buffer solution and oscillating;
(5) washing: and (4) replacing and washing the soaked hydrogel with deionized water.
2. The method of claim 1, wherein step (1) is performed in a manner corresponding to step 100mL of water, ZrOCl2·8H2The dosage of O is 2-4g, and the dosage of agarose powder is 1-2 g.
3. The method of claim 2, wherein in step (4), the MES buffer solution has a pH of 6.7-6.8; the soaking time is 1.5-3 hours.
4. The method of claim 3, wherein the step (5) is carried out until the pH value of the deionized water solution after washing is 5.6 ± 0.3.
5. An adsorbent film for a DGT device, prepared by the method of any one of claims 1 to 4.
6. A DGT device comprising an adsorbent film as claimed in claim 5.
7. Use of a DGT device as claimed in claim 6 for the detection of oxidising anions in water, sediment or soil.
8. Use of a DGT device according to claim 7, characterised in that it comprises the steps of:
(1) putting in the device: putting the device in water, soil or sediment, and enriching for a certain time;
(2) recovering the device: taking out the DGT device and thoroughly cleaning the surface of the device;
(3) the device develops color: putting the device or the adsorption film into a color developing agent for color development;
(4) analysis and data processing: after the color development is completed, the data is analyzed and processed.
9. Use of a DGT device as claimed in claim 8, characterised in that the analysis and data processing in step (4) is performed in conjunction with CID techniques.
10. Use of a DGT device according to claim 9, characterised in that said combining with CID techniques comprises the steps of:
(1) shaking the surface of the washing device;
(2) taking out the adsorption film or placing the device on an office or household flat-panel scanner to scan and store the color development surface; or when the sample amount is small, scanning and storing by using a handheld color difference meter;
(3) the color was converted to gray using ImageJ software and quantitative calculations were performed using a standard curve.
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| CN111992189A (en) * | 2020-08-28 | 2020-11-27 | 南京维申环保科技有限公司 | Adsorption film for biomembrane DGT device, preparation method and application |
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