CN113960021A - Test paper for rapidly detecting mercury ions by nano silver particles based on green synthesis - Google Patents
Test paper for rapidly detecting mercury ions by nano silver particles based on green synthesis Download PDFInfo
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- CN113960021A CN113960021A CN202010629448.5A CN202010629448A CN113960021A CN 113960021 A CN113960021 A CN 113960021A CN 202010629448 A CN202010629448 A CN 202010629448A CN 113960021 A CN113960021 A CN 113960021A
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- 238000012360 testing method Methods 0.000 title claims abstract description 33
- 229910052753 mercury Inorganic materials 0.000 title claims abstract description 32
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 31
- -1 mercury ions Chemical class 0.000 title claims abstract description 30
- 239000002245 particle Substances 0.000 title claims abstract description 10
- 230000015572 biosynthetic process Effects 0.000 title description 4
- 238000003786 synthesis reaction Methods 0.000 title description 4
- BQPIGGFYSBELGY-UHFFFAOYSA-N mercury(2+) Chemical compound [Hg+2] BQPIGGFYSBELGY-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 9
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 8
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 4
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 3
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 19
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 6
- 230000008859 change Effects 0.000 claims description 5
- 229910052709 silver Inorganic materials 0.000 claims description 5
- 239000004332 silver Substances 0.000 claims description 5
- 229920005552 sodium lignosulfonate Polymers 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000011981 development test Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 3
- 239000012490 blank solution Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 12
- 229920005610 lignin Polymers 0.000 abstract description 11
- 230000000007 visual effect Effects 0.000 abstract description 3
- 239000003381 stabilizer Substances 0.000 abstract description 2
- 239000003638 chemical reducing agent Substances 0.000 abstract 1
- 238000002791 soaking Methods 0.000 abstract 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 11
- 238000010521 absorption reaction Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- 238000004566 IR spectroscopy Methods 0.000 description 1
- 235000000069 L-ascorbic acid Nutrition 0.000 description 1
- 239000002211 L-ascorbic acid Substances 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000002795 fluorescence method Methods 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229940008718 metallic mercury Drugs 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 238000009597 pregnancy test Methods 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000012549 training Methods 0.000 description 1
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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
- G01N21/75—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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y15/00—Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
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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
- G01N21/75—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
- G01N2021/7756—Sensor type
- G01N2021/7759—Dipstick; Test strip
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- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Nanotechnology (AREA)
- Analytical Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Plasma & Fusion (AREA)
- Molecular Biology (AREA)
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Abstract
The invention relates to a test paper for rapidly detecting mercury ions based on green synthesized nano silver particles, which is prepared by soaking common filter paper in a nano silver solution, wherein the nano silver is prepared from green stabilizer lignin and a green reducing agent ascorbic acid. The test paper has visual mercury ion detection result, is simple to operate, is environment-friendly and environment-friendly, and can be used for detecting mercury ions in actual samples. The method provided by the invention can accurately and quickly detect mercury ions.
Description
Technical Field
The invention belongs to the technical field of rapid detection and analysis, and particularly relates to green synthesized test paper for rapidly detecting mercury ions by nano silver particles.
Background
Metallic mercury is a highly toxic global environmental pollutant, and due to its characteristics of high migration, non-degradability, bio-enrichment and food chain amplification, even if present in trace amounts in the environment, it poses a great threat to the health of animals, plants and human beings. Mercury exists in the environment in a variety of forms, with water-soluble mercury ions being one of the most common and stable forms of mercury contamination. The traditional mercury ion detection method mainly comprises an atomic absorption method, an atomic fluorescence method, a high performance liquid chromatography method, inductive coupling and the like. Although relatively accurate detection results can be obtained, the technologies rely on large-scale instruments and equipment, consume time and have high detection cost, and the requirements of rapid detection on production sites are difficult to meet. Therefore, a simple, rapid, economical and accurate mercury ion detection and analysis method is urgently needed. The color development test paper detection technology is a rapid detection technology developed in the early 80 s of the 20 th century, and is widely applied to the technical field of rapid detection due to the obvious advantages of rapidness, sensitivity, low cost and the like. The test paper method has wide application at present because the test paper is simple, convenient, quick, economic, does not need professional training and the like. The advantages of the test paper make the test paper more and more popular, and the test paper covers various aspects of medical treatment, environment, food and the like. The widely and commonly used test paper products in the market at present mainly comprise blood glucose test paper, pH test paper, early pregnancy test paper, starch test paper and the like, which are closely related to the life of people, and bring convenience to the life of people.
Disclosure of Invention
The invention provides simple and accurate test paper for rapidly detecting mercury ions based on green synthesized nano silver particles, which is used for rapidly and visually detecting mercury ions and proves that the test paper is visual and has strong operability.
A method for detecting mercury ions based on green synthesized nano silver particles comprises the following specific steps:
0.30g of sodium lignosulfonate was weighed accurately and placed in a 250mL round bottom flask, dissolved in 30mL of water and magnetically stirred at room temperature for 3 min. Then 30mL of 0.01mol/L silver nitrate solution and 30mL of 1mg/mL ascorbic acid solution are added, and after 5 hours of reaction at 37 ℃, the solution changes from brown to yellow to obtain silver nano solution for later use.
The lignin-stabilized silver nanoparticles prepared by the green synthesis method are flaky, the silver nanoparticles are flaky, and the transmission electron microscope can more remarkably see that the nano silver is spherical (fig. 2c and d), the diameter of the silver nanoparticles is about 20 nm, and the silver nanoparticles are uniformly distributed. The lattice spacing was 0.1192 nm. Proves that the lignin plays a role of a bracket in the reaction, also plays a good dispersing role and gives full play to the advantages of the lignin.
The infrared spectrum characterization is carried out on the lignin, the nano silver and the nano silver added with mercury ions, and as shown in figure 3a, the infrared characteristic peak of the lignin can be seen: 3437cm-12929cm at the peak of stretching vibration of-OH-1The peak of (A) is-CH in the aromatic ring3Stretching vibration peak of 1611, 1523 and 1388cm-1The peak is the absorption peak of the aromatic ring skeleton, 1345cm-1The peak is syringyl ring C = O stretching vibration absorption peak, 1137cm-1Is C-O-C stretching vibration absorption peak, 1038 cm-12850cm as C-C stretching vibration absorption peak-1Is located at-CH stretching vibration peak, 620cm-1Is a strong absorption peak of-C ≡ CH. The comparison shows that the structure of the lignin is not changed by the prepared nano silver and the nano silver added with mercury ions. Comparison shows that the lignin group is not greatly changed after the reaction, which is consistent with an infrared spectrogram, and proves that the lignin mainly plays a role of a stabilizer and a dispersant.
Comparing the X-ray diffraction spectrogram, wherein the ratio of nano silver in the spectrogram: five peaks at 2 θ =38.12 °, 44.2 °, 64.37 °, 77.50 ° and 81.38 °, which are identical to JCPDS (nos. 89-3722), correspond to lattice planes of (111), (200), (220), (311), (222) Ag, which is consistent with the information reported for crystalline silver nanoparticles. The method can prepare high-purity silver nanoparticles. After the mercury ions are added, as can be seen from fig. 3a, the lignin structure as the nano silver ligand is not significantly changed after the mercury ions are added, which indicates that the mercury ions do not destroy the lignin structure. Fig. 3b shows that the peak of lignin is unchanged after the mercury ions are added, which is consistent with the conclusion of infrared spectroscopy, while the single-crystal spectrogram of the silver simple substance in the nano silver is greatly changed, which indicates that the mercury ions may interact with silver.
Mercury ion solutions with different concentrations are sequentially added into the nano-silver solution, the color of the nano-silver solution gradually becomes lighter along with the increase of the mercury ion content in the system, the color changes from bright yellow to light yellow, and the whole system is nearly colorless when the mercury ion content in the system reaches 70 micromoles (as shown in figure 4 a).
Fig. 4b shows that the filter paper soaked with the nano silver solution is naturally dried to prepare the color test paper, and the blank solution and the six mercury ion solutions with different concentrations are respectively added dropwise, so that the white area in the liquid ring of the color test paper is gradually enlarged along with the addition of the mercury ion concentration, and the content of the mercury ions can be quickly judged through the color change of the color test paper.
The test paper is rapid, accurate and visual in mercury ion detection, the preparation process of the test paper is simple, all reagents are safe and environment-friendly, and the test paper is a method for rapidly detecting mercury ions in actual samples.
The green synthesis-based test paper for rapidly detecting mercury ions by using nano silver particles has high selectivity. Under the same conditions, interfering ions (Cu) possibly existing in actual water samples are used2+、Al3+、Ce3+、Cr6+、Zr4+、Na+、Ca2+、Pb2+、Ni+、Mn2+、K+、Fe2+、Zn2+、La3+、Mg2+) The obvious absorbance change of the silver nanoparticles is not caused when the silver nanoparticles are dripped into the silver nanoparticle solution, which shows that the method has high selectivity for detecting mercury ions.
Drawings
FIG. 1 is a schematic diagram of detection of mercury ions by silver nanoparticles.
FIG. 2 is a scanning electron microscope and a transmission electron microscope image of silver nanoparticles.
Fig. 3 XRD and IR patterns of silver nanoparticles.
FIG. 4 is a color contrast diagram of test paper for detecting ions.
FIG. 5 is a graph of a selective experiment.
Detailed Description
Example 1.
The embodiments of the present invention will be described in detail below. It should be emphasized that the following description of the embodiments is merely exemplary and is not intended to limit the scope and application of the present invention.
A test paper for rapidly detecting mercury ions by nano silver particles based on green synthesis comprises the following specific operation steps:
after 0.3g of sodium lignosulfonate, which was weighed, was added to a 250mL round bottom flask, 30mL of purified water was added and magnetic stirring was performed at room temperature for 3 min. Then, while maintaining the temperature at 37 ℃. + -. 1 ℃, 30mL of a 0.01mol/L silver nitrate solution was added to the round-bottomed flask, followed by 30mL of a 1mol/L ascorbic acid solution, and after magnetically stirring for 5 hours, the heating was stopped, and the sample was stored at 4 ℃.
Claims (2)
1. The test paper for rapidly detecting the mercury ions based on the green synthesized nano silver particles is characterized in that the mercury ions are dripped onto the test paper soaked in the nano silver solution to cause the color change of the test paper, and the color change of the test paper is obvious along with the increase of the concentration of the dripped mercury ions, so that the test paper for rapidly detecting the mercury ions is designed;
the method comprises the following specific steps:
(1) preparation of nano silver
Accurately weighing 0.30g of sodium lignosulfonate, placing the sodium lignosulfonate in a 250mL round-bottom flask, adding 30mL of water for dissolving, magnetically stirring for 3min at room temperature, adding 30mL of 0.01mol/L silver nitrate solution and 30mL of 1mg/mL ascorbic acid solution, reacting at 37 ℃ for 5 hours, and changing the color of the solution from brown to yellow to obtain silver nano solution for later use;
(2) preparation of test paper
And (3) the filter paper soaked in the nano silver solution is naturally dried to prepare a color development test paper, a blank solution and mercury ion solutions with different concentrations are respectively dripped into the test paper, and the color change of the color development test paper is observed, so that the mercury ions are rapidly detected.
2. The test paper for rapidly detecting mercury ions based on green synthesized nano silver particles as claimed in claim 1, wherein: the mercury ions in the actual sample can be detected visually and rapidly.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010629448.5A CN113960021A (en) | 2020-07-03 | 2020-07-03 | Test paper for rapidly detecting mercury ions by nano silver particles based on green synthesis |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010629448.5A CN113960021A (en) | 2020-07-03 | 2020-07-03 | Test paper for rapidly detecting mercury ions by nano silver particles based on green synthesis |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102489716A (en) * | 2011-12-15 | 2012-06-13 | 湖南科技大学 | Preparation method for lignosulfonate nano-silver colloid |
| CN103808717A (en) * | 2014-02-14 | 2014-05-21 | 哈尔滨师范大学 | Method for detecting mercury ions by adopting colorimetric method |
| CN103884669A (en) * | 2014-03-31 | 2014-06-25 | 湖南大学 | Preparation method and application of nano-silver probe for detecting mercury ions |
| KR20180082704A (en) * | 2017-01-10 | 2018-07-19 | 한국기초과학지원연구원 | Mercury concentration measurement sensor and Mercury concentration measurement method |
-
2020
- 2020-07-03 CN CN202010629448.5A patent/CN113960021A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102489716A (en) * | 2011-12-15 | 2012-06-13 | 湖南科技大学 | Preparation method for lignosulfonate nano-silver colloid |
| CN103808717A (en) * | 2014-02-14 | 2014-05-21 | 哈尔滨师范大学 | Method for detecting mercury ions by adopting colorimetric method |
| CN103884669A (en) * | 2014-03-31 | 2014-06-25 | 湖南大学 | Preparation method and application of nano-silver probe for detecting mercury ions |
| KR20180082704A (en) * | 2017-01-10 | 2018-07-19 | 한국기초과학지원연구원 | Mercury concentration measurement sensor and Mercury concentration measurement method |
Non-Patent Citations (1)
| Title |
|---|
| 李红红 等: "纳米金银材料在比色检测汞中的应用", 岩矿测试, vol. 31, no. 5, pages 757 - 766 * |
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