CN114184606B - Preparation and application methods of mercury ion on-site rapid detection material - Google Patents
Preparation and application methods of mercury ion on-site rapid detection material Download PDFInfo
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- CN114184606B CN114184606B CN202111427691.XA CN202111427691A CN114184606B CN 114184606 B CN114184606 B CN 114184606B CN 202111427691 A CN202111427691 A CN 202111427691A CN 114184606 B CN114184606 B CN 114184606B
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- 239000000463 material Substances 0.000 title claims abstract description 44
- 238000001514 detection method Methods 0.000 title claims abstract description 34
- BQPIGGFYSBELGY-UHFFFAOYSA-N mercury(2+) Chemical compound [Hg+2] BQPIGGFYSBELGY-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 229910052753 mercury Inorganic materials 0.000 claims abstract description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- -1 mercury ions Chemical class 0.000 claims abstract description 25
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims abstract description 4
- DBCAQXHNJOFNGC-UHFFFAOYSA-N 4-bromo-1,1,1-trifluorobutane Chemical compound FC(F)(F)CCCBr DBCAQXHNJOFNGC-UHFFFAOYSA-N 0.000 claims abstract description 4
- RCTYPNKXASFOBE-UHFFFAOYSA-M chloromercury Chemical compound [Hg]Cl RCTYPNKXASFOBE-UHFFFAOYSA-M 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 4
- STVZJERGLQHEKB-UHFFFAOYSA-N ethylene glycol dimethacrylate Substances CC(=C)C(=O)OCCOC(=O)C(C)=C STVZJERGLQHEKB-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 4
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 14
- 238000006116 polymerization reaction Methods 0.000 claims description 11
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 230000008859 change Effects 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 238000010521 absorption reaction Methods 0.000 claims description 5
- 239000003431 cross linking reagent Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000000178 monomer Substances 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 3
- 239000012498 ultrapure water Substances 0.000 claims description 3
- 230000010355 oscillation Effects 0.000 claims description 2
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 6
- 238000001308 synthesis method Methods 0.000 abstract description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 229910052760 oxygen Inorganic materials 0.000 abstract 1
- 239000001301 oxygen Substances 0.000 abstract 1
- 239000013077 target material Substances 0.000 abstract 1
- 150000002500 ions Chemical class 0.000 description 15
- 238000001179 sorption measurement Methods 0.000 description 13
- 239000000523 sample Substances 0.000 description 10
- 229910021645 metal ion Inorganic materials 0.000 description 7
- 238000011161 development Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- 239000013522 chelant Substances 0.000 description 2
- 238000012764 semi-quantitative analysis Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 1
- 231100000693 bioaccumulation Toxicity 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002795 fluorescence method Methods 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 238000000918 plasma mass spectrometry Methods 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 239000003361 porogen Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 231100001234 toxic pollutant Toxicity 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
Classifications
-
- 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
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
-
- 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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
-
- 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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N2021/0106—General arrangement of respective parts
- G01N2021/0112—Apparatus in one mechanical, optical or electronic block
Abstract
The invention belongs to the technical field of rapid detection of heavy metals, and discloses a preparation and application method of a mercury ion on-site rapid detection material. The preparation method comprises the following steps: combining thiomilone with HgCl 2 Dissolving in proper amount of ethanol in a ratio of 4:1, performing ultrasonic treatment until the ethanol is completely dissolved, and stirring and prepolymerizing for 2h at room temperature; adding ethylene glycol dimethacrylate and azodiisobutyronitrile into the solution, fully dissolving and mixing, and then adding toluene; adding sodium dodecyl benzene sulfonate solution, and oscillating for 12h at 70 ℃ under the condition of introducing N2 and no oxygen; washing the product, eluting mercury ions, and drying to obtain the target material. The synthesis method of the mercury ion on-site rapid detection material provided by the invention is simple and easy to implement and has low cost; the material can be used for on-site detection of mercury ion concentration in water, and is simple and rapid, easy to use, strong in anti-interference capability and reliable in result.
Description
Technical Field
The invention belongs to the technical field of rapid detection of heavy metal ions, and relates to a mercury ion (Hg) 2+ ) The preparation and application methods of the rapid detection material on site.
Technical Field
Mercury is a highly toxic pollutant which can not be degraded and can migrate in the environment, and the toxicity has the characteristics of durability, bioaccumulation and the like, and the famous "water disease" is caused by people eating fishes in mercury polluted water. Mercury contaminants in industrial wastewater are mainly discharged in the form of inorganic mercury. In order to strictly control the content of mercury in water environment, national integrated wastewater discharge Standard GB 8978-1996 prescribes that the maximum allowable discharge concentration of total mercury in wastewater is 0.05mg L -1 。
Currently, there are various detection techniques for metal ions, and there are commonly used atomic absorption methods, atomic emission methods, atomic fluorescence methods, plasma mass spectrometry, and the like. These techniques are sensitive and accurate, but require high precision instrumentation, are costly, are complex to operate, and can only be used for laboratory detection. In addition, a series of pretreatment is sometimes required, and the process is cumbersome and time-consuming.
The existing metal ion rapid detection technology such as rapid detection test paper, rapid detection kit and the like generally has the problems of low sensitivity, multiple interference factors and the like. Particularly for the elements with low content in the water body such as mercury, the elements with high concentration are greatly disturbed by other elements with high concentration, the sensitivity is not high enough,usually more than 1mg L -1 Can be detected and can not meet the requirements of sewage discharge management. Therefore, a technology for detecting trace mercury ions in water on site with high response speed, high sensitivity and high accuracy needs to be developed.
Ion Imprinted Polymers (IIPs) are a highly selective adsorbent material developed in recent years. Prepolymerizing through the interaction of template ions and functional monomers, and then forming a polymer in the presence of a crosslinking agent and a porogen; and after the template ions are eluted and removed, obtaining the ion imprinted polymer capable of specifically recognizing the target ions. The IIPs are used for adsorbing ions to be detected in the sample solution, so that the target ions can be concentrated, and the influence of coexisting ions in the sample can be relieved to a great extent.
Heavy metal ions bind to the chelating agent, typically yielding a colored chelate. In a certain concentration range, the color of the chelate is positively correlated with the concentration of heavy metal ions. Therefore, the change degree of the color of the material can be distinguished by naked eyes to perform semi-quantitative analysis on heavy metal ions.
Disclosure of Invention
In view of the several disadvantages of the existing mercury ion rapid detection technology, the invention provides a mercury ion (Hg) 2+ ) The preparation method of the on-site rapid detection material comprises the following steps:
(1) Combining thiomilone with HgCl 2 Dissolving in ethanol at a molar ratio of 4:1, performing ultrasonic treatment until the solution is completely dissolved, and stirring and prepolymerizing for 2h at room temperature; 42mmol of ethylene glycol dimethacrylate and 0.1g of azodiisobutyronitrile are added into the solution after the prepolymerization, and toluene is added after the mixture is fully dissolved and mixed;
(2) Preparing 70mL of sodium dodecyl benzene sulfonate solution, adding the sodium dodecyl benzene sulfonate solution into the solution obtained in the step (1), introducing nitrogen for 20min to deoxidize, and carrying out oscillation polymerization for 12h at 70 ℃ to obtain a polymerization product;
(3) Washing the polymerization product obtained in the step (2) with methanol until the polymerization product is clear so as to wash out unreacted functional monomers and cross-linking agents; eluting with HCl solution to remove template mercury ions until mercury ions cannot be detected by cold atom absorption mercury detector; and then washing with ultra-pure water for three times, and drying at 50 ℃ to obtain the mercury ion on-site rapid detection material.
In addition, the invention also comprises a rapid and sensitive on-site detection method of mercury ions in water, the method is based on the prepared rapid detection material of mercury ions, and the concentration of mercury ions is analyzed semi-quantitatively by distinguishing the change degree of colors before and after the material contacts with a water sample, and the specific implementation method is as follows:
(1) Adding 100mg of mercury ion on-site rapid detection material into 10mL of water sample before detection, shaking for 30s, standing for 3min, and waiting for the color change of the material;
(2) And comparing the color displayed by the material with the standard color level of mercury ions, and analyzing the concentration of mercury ions in the sample.
Compared with the prior art, the invention has the following advantages:
(1) The synthesis method of the mercury ion on-site rapid detection material provided by the invention has the advantages of readily available raw materials, simplicity and convenience in method and lower cost.
(2) The on-site rapid detection method for the concentration of mercury ions in the water body is simple to operate, does not need to add other reagents, and is high in anti-interference capability, stable in result and basically consistent with the detection result of an instrument.
(3) The mercury ion on-site rapid detection material provided by the invention can be recycled for 5 times.
Detailed Description
The invention will be further described with reference to the following specific embodiments, but the examples are not intended to limit the invention in any way.
Example 1
(1) Combining thiomilone with HgCl 2 Dissolving in ethanol at a molar ratio of 4:1, performing ultrasonic treatment until the solution is completely dissolved, and stirring and prepolymerizing for 2h at room temperature; 42mmol of ethylene glycol dimethacrylate and 0.1g of azodiisobutyronitrile are added into the solution after the prepolymerization, and toluene is added after the mixture is fully dissolved and mixed;
(2) Preparing 70ml of sodium dodecyl benzene sulfonate solution, adding the sodium dodecyl benzene sulfonate solution into the solution obtained in the step (1), introducing nitrogen for 20min to deoxidize, and oscillating and polymerizing for 12h at 70 ℃ to obtain a polymerization product;
(3) Washing the polymerization product obtained in the step (2) with methanol until the polymerization product is clear so as to wash out unreacted functional monomers and cross-linking agents; eluting with HCl solution to remove template mercury ions until mercury ions cannot be detected by cold atom absorption mercury detector; and then washing with ultra-pure water for three times, and drying at 50 ℃ to obtain the mercury ion on-site rapid detection material.
Example 2
Simulating the existence of various heavy metal ions in an actual water body, and using metal ions Zn which have similar property and structure and possibly cause interference 2+ 、Cd 2+ 、Ni 2+ 、Pb 2+ 、Cu 2+ Performing competitive adsorption experiments, wherein the concentration of each metal is 100mg L under identical adsorption conditions except for different metal ions -1 。
The results show that the material does not change in color when it encounters various interfering metal ions, and only changes in color when it contacts a mercury-containing aqueous sample.
Calculating the distribution coefficient K of the material by the following formula d (mL g -1 ) Selective blotting coefficient α:
wherein Q is e And C e K is the adsorption quantity and concentration of metal ions in the solution adsorption balance d1 、K d2 The partition coefficients of mercury ions and other competing ions, respectively.
Calculation shows that the Hg is the material pair 2+ The adsorption quantity of (C) is 8.89mg g -1 The imprinting coefficients for the other metal ions are 4.99, 6.71, 3.85, 5.25, 7.96, respectively, which are significantly higher than those of the other ions.
100mg of material was added to 50mL, pH 4, and concentration 100mg L -1 The adsorption performance was measured at different adsorption times (1-300 min) and the temperature was controlled at 25 ℃.The results show that the adsorption reaches equilibrium at 120min and accords with a quasi-secondary kinetic adsorption model.
100mg of the material is added into 50mL of mercury ion solution with different initial concentrations, the material is absorbed by shaking at 25 ℃ for 120min, and an adsorption isotherm is drawn according to the obtained result. The results show that the adsorption of mercury ions by the material accords with a Langmuir adsorption model.
And carrying out adsorption-desorption experiments on the material, and determining the renewable performance of the material. The results show that the adsorption performance of the material is not obviously reduced after the material is repeatedly used for 5 times.
Example 3
The on-site rapid detection material for mercury ions is used for measuring the mercury ions in an environmental water sample. Collecting water samples such as river water, lake water and the like, wherein the pH value is about 7, and adding mercury ions into the water samples by using a standard adding method. 100mg of material was added to 10mL of water sample, and after shaking for 30s, the mixture was allowed to stand, and after three minutes, the color change of the material was observed. The color development of the materials in water samples with different mercury addition amounts is shown in the following table 1. And (3) comparing the color of the material with the standard color level of mercury ions, and performing semi-quantitative analysis on the concentration of mercury ions in the water sample. It can be seen that the color development detection result is basically consistent with the measurement result of the cold atom absorption mercury porosimeter, and the accuracy is high. In a plurality of parallel experiments, the material has stable color development and good reproducibility.
Table 1 material and instrument for detecting and analyzing mercury ions in actual water sample
The above examples verify the reliability of the present invention in practical water sample application, and the embodiments of the present invention are not limited to the above forms, and any other changes, modifications, substitutions, combinations, and simplifications made without departing from the spirit and principles of the present invention should be equivalent substitution, and are included in the scope of the present invention.
Claims (3)
1. The preparation method of the mercury ion on-site rapid detection material is characterized by comprising the following steps of:
(1) Combining thiomilone with HgCl 2 Dissolving in ethanol solution at a molar ratio of 4:1, performing ultrasonic treatment until the solution is completely dissolved, and stirring and prepolymerizing for 2h at room temperature; 42mmol of ethylene glycol dimethacrylate and 0.1g of azodiisobutyronitrile are added into the solution after the prepolymerization, and toluene solution is added after the mixture is fully dissolved and mixed;
(2) Preparing 70mL of sodium dodecyl benzene sulfonate solution, adding the sodium dodecyl benzene sulfonate solution into the solution obtained in the step (1), introducing nitrogen for 20min to deoxidize, and carrying out oscillation polymerization for 12h at 70 ℃ to obtain a polymerization product;
(3) Washing the polymerization product obtained in the step (2) with methanol until the polymerization product is clear so as to remove unreacted functional monomers and cross-linking agents; eluting with HCl solution to remove template mercury ions until mercury ions cannot be detected by cold atom absorption mercury detector; and then washing with ultrapure water for three times, and drying at 50 ℃ to obtain the mercury ion on-site rapid detection material.
2. A mercury ion on-site rapid detection material prepared by the preparation method of claim 1.
3. A method for determining the concentration of mercury ions in a body of water based on the mercury ion on-site rapid detection material of claim 2, comprising the steps of:
(1) Adding 100mg of mercury ion on-site rapid detection material into 10mL of water sample before detection, and waiting for color change of the material after shaking for 30 s; for 1mg L -1 The mercury-containing water sample can be used for observing the color change of the material within 1 min; for 1mg L -1 The following is 0.05mg L -1 The water sample needs to wait for about 3 minutes;
(2) And comparing the color displayed by the mercury ion on-site rapid detection material with the standard color level of the mercury ions, and analyzing the concentration of the mercury ions in the water sample.
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| CN202111427691.XA CN114184606B (en) | 2021-11-26 | 2021-11-26 | Preparation and application methods of mercury ion on-site rapid detection material |
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| CN114184606B true CN114184606B (en) | 2024-01-16 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103087346A (en) * | 2013-01-29 | 2013-05-08 | 温州市质量技术监督检测院 | Preparation method of blotting membrane for Hg<2+> detection |
| CN104140530A (en) * | 2014-07-22 | 2014-11-12 | 中国科学院烟台海岸带研究所 | Mercury ion imprinted polymer and method and application thereof |
| CN104844758A (en) * | 2015-04-16 | 2015-08-19 | 浙江普正检测技术有限公司 | Mercury ion imprinting polymer and preparation method thereof |
| CN112730394A (en) * | 2020-12-17 | 2021-04-30 | 广东工业大学 | Copper ion rapid color development detection ion imprinting material and preparation method and application thereof |
| CN113405992A (en) * | 2021-06-22 | 2021-09-17 | 江南大学 | Method for detecting heavy metal ions by combining complexing colorimetric array microfluidic paper chip with smart phone |
-
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- 2021-11-26 CN CN202111427691.XA patent/CN114184606B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103087346A (en) * | 2013-01-29 | 2013-05-08 | 温州市质量技术监督检测院 | Preparation method of blotting membrane for Hg<2+> detection |
| CN104140530A (en) * | 2014-07-22 | 2014-11-12 | 中国科学院烟台海岸带研究所 | Mercury ion imprinted polymer and method and application thereof |
| CN104844758A (en) * | 2015-04-16 | 2015-08-19 | 浙江普正检测技术有限公司 | Mercury ion imprinting polymer and preparation method thereof |
| CN112730394A (en) * | 2020-12-17 | 2021-04-30 | 广东工业大学 | Copper ion rapid color development detection ion imprinting material and preparation method and application thereof |
| CN113405992A (en) * | 2021-06-22 | 2021-09-17 | 江南大学 | Method for detecting heavy metal ions by combining complexing colorimetric array microfluidic paper chip with smart phone |
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