CN106442515B - A kind of visual quantitative detecting method of simple silver ion - Google Patents
A kind of visual quantitative detecting method of simple silver ion Download PDFInfo
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- CN106442515B CN106442515B CN201611039050.6A CN201611039050A CN106442515B CN 106442515 B CN106442515 B CN 106442515B CN 201611039050 A CN201611039050 A CN 201611039050A CN 106442515 B CN106442515 B CN 106442515B
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- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 25
- 230000000007 visual effect Effects 0.000 title claims abstract description 21
- 239000000243 solution Substances 0.000 claims abstract description 36
- 239000007864 aqueous solution Substances 0.000 claims abstract description 20
- 238000001514 detection method Methods 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000004458 analytical method Methods 0.000 claims abstract description 8
- 239000003960 organic solvent Substances 0.000 claims abstract description 8
- 230000002596 correlated effect Effects 0.000 claims abstract description 4
- 238000012360 testing method Methods 0.000 claims description 12
- 229920003023 plastic Polymers 0.000 claims description 4
- 239000004033 plastic Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 3
- CMZYGFLOKOQMKF-UHFFFAOYSA-N 1-(3,5-dimethylphenyl)-3,5-dimethylbenzene Chemical group CC1=CC(C)=CC(C=2C=C(C)C=C(C)C=2)=C1 CMZYGFLOKOQMKF-UHFFFAOYSA-N 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- HFACYLZERDEVSX-UHFFFAOYSA-N benzidine Chemical compound C1=CC(N)=CC=C1C1=CC=C(N)C=C1 HFACYLZERDEVSX-UHFFFAOYSA-N 0.000 abstract description 13
- 239000011259 mixed solution Substances 0.000 abstract description 4
- UAIUNKRWKOVEES-UHFFFAOYSA-N 3,3',5,5'-tetramethylbenzidine Chemical compound CC1=C(N)C(C)=CC(C=2C=C(C)C(N)=C(C)C=2)=C1 UAIUNKRWKOVEES-UHFFFAOYSA-N 0.000 abstract description 3
- 238000003556 assay Methods 0.000 abstract description 3
- 238000002474 experimental method Methods 0.000 abstract description 3
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 7
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 6
- 150000002500 ions Chemical class 0.000 description 5
- 239000012496 blank sample Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 239000000523 sample Substances 0.000 description 4
- 229910021642 ultra pure water Inorganic materials 0.000 description 3
- 239000012498 ultrapure water Substances 0.000 description 3
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 2
- 239000012491 analyte Substances 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 239000012074 organic phase Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 241000669003 Aspidiotus destructor Species 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 241001062009 Indigofera Species 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- 238000004847 absorption spectroscopy Methods 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000003125 aqueous solvent Substances 0.000 description 1
- DMVOXQPQNTYEKQ-UHFFFAOYSA-N biphenyl-4-amine Chemical compound C1=CC(N)=CC=C1C1=CC=CC=C1 DMVOXQPQNTYEKQ-UHFFFAOYSA-N 0.000 description 1
- 230000000875 corresponding effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 150000002460 imidazoles Chemical class 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000013507 mapping Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 102000039446 nucleic acids Human genes 0.000 description 1
- 108020004707 nucleic acids Proteins 0.000 description 1
- 150000007523 nucleic acids Chemical class 0.000 description 1
- 238000012123 point-of-care testing Methods 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Plasma & Fusion (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
- Optical Measuring Cells (AREA)
Abstract
The invention discloses a kind of simple visual quantitative detecting methods of silver ion.This method using can the organic solvent of miscible with water and 25 DEG C of lower densities density for being greater than water dissolve 3,3', 5,5'- tetramethyl benzidine (TMB).When that will be added dropwise containing the aqueous solution of silver ion into TMB solution, Ag+Quickly oxidation TMB generates blue quinoid benzidine.Since used organic solvent can be used as the intelligent regulator of double-colored layering, the colourless double-colored mixed solution of unique upper layer blue-lower layer, and the size and Ag of the blue solution length are finally obtained+Concentration be positively correlated, thus by macroscopic visual observation, measure blue solution length micromolar levels Ag can be realized+Quantitative detection.Ag in the method for the present invention+Detection process is extremely simple, non-pro operator can also carry out experiment, more importantly it can carry out quantifiable signal reading without using any instrument or equipment, the field assay that sample is also able to achieve while greatly reducing analysis cost and detection immediately.
Description
Technical field
The invention belongs to heavy metal ion chemical sensitisation detection technique fields, and in particular to a kind of simple silver ion is visual
Quantitative detecting method.
Background technique
Silver ion (Ag+) it is widely used in photography, image, electric appliance, medicine and other fields.But Ag+Ion can pass through food chain richness
Combine in human body, the activity of such heavy metal ion energy destructive enzyme of high concentration, and can be with amine, imidazoles, the carboxylic of various metabolins
The functional groups such as base combine, and seriously affect, damage the health of the mankind, even result in death.Ag traditional at present+Quantitative detection side
Method mainly includes atom and ultraviolet absorption spectroscopy, fluorescent spectrometry, mass spectrography, electrochemical sensor method, ion selectivity electricity
Pole method etc..However, these methods based on spectrometer, mass spectrograph and electrochemical electrode exist to some extent analysis cost compared with
Height, cumbersome time-consuming, more demanding to the operator professional skill of analytic process, used instrument price are expensive and volume is huge
Greatly, field assay and the immediately series of problems such as detection (Point-of-Care Testing) be cannot be used for.
Summary of the invention
In view of the deficiencies of the prior art, it is an object of the present invention to provide a kind of simple visual quantitative detection sides of silver ion
Method.
Thinking of the invention: researches show that silver ion (Ag in aqueous solution+) can be by 3,3', 5,5'- tetramethyl benzidine
(TMB) colorimetric probe, which quickly aoxidizes, generates quinoid benzidine product, obtains the uniform blue aqueous solution of color.It is used in the present invention
The organic solvent that miscible with water and density is greater than the density (25 DEG C) of water dissolves TMB probe.When by Ag+Aqueous solution, which is added dropwise, enters this
When in class TMB solution, a degree of exchange, Ag occur for the solute in two kinds of solution+Quickly oxidation TMB generates quinoid biphenyl
Amine.Because the quinoid benzidine product is more likely to be formed in water phase, it is colourless to finally obtain unique upper layer blue-lower layer
Double-colored mixed solution.Upper layer is mainly the lesser water phase of density, and blue is presented because containing quinoid benzidine product;Lower layer master
To be the biggish organic phase of density, and present because there is no quinoid benzidine product or the production concentration too low colourless.More attach most importance to
It wants, institute can be further used as the intelligent regulator of double-colored layering using organic solvent." intelligence " refers to Ag+The increasing of concentration
Greatly, the length of colored solutions increases with it in finally formed double-colored mixed solution.Therefore, it is not needing using any professional instrument
In the case where device or equipment, Ag can be realized only by the length of macroscopic visual observation, measurement colored solutions+Quantitative inspection
It surveys.
Specific steps are as follows:
Step 1 will contain Ag+Aqueous solution be added drop-wise to equipped with 3,3', 5,5'- tetramethyl benzidine (TMB) solution it is saturating
In bright test tube.
Step 2, macroscopic visual observation, the length for measuring cuvette blue solution at the middle and upper levels, the size and Ag of the length+Concentration is positively correlated, i.e. completion Ag+Visual quantitative detection.
It is described to contain Ag+Aqueous solution in Ag+For target analytes or by chemical reaction and biological respinse generate two
Grade analyte.
The solvent of described 3,3', 5,5'- tetramethyl biphenyl amine aqueous solutions is organic solvent, and the organic solvent is miscible with water and 25
DEG C lower density is greater than the density of water.
The cuvette is that the graduated cuvette of outer wall or outer wall do not have graduated cuvette, cuvette
Material is plastics or glass;When the outer wall of cuvette has scale, the length for measuring cuvette blue solution at the middle and upper levels is
It is completed by directly reading the scale on cuvette outer wall relevant to blue solution length;When the outer wall of cuvette does not have
When having scale, measuring cuvette, the length of blue solution is to measure examination on cuvette outer wall by using ruler at the middle and upper levels
The length of blue solution is completed in pipe.
With existing Ag+Ion quantitative detecting method is compared, and of the invention has the prominent advantages that: 1) Ag+Detection process is extremely
Simply, non-pro operator can also carry out experiment;2) any instrument or equipment are not used, only by using ruler
Colored solutions length is measured from test tube outer wall or directly reads the scale on test tube outer wall relevant to colored solutions length
Quantifiable signal reading is carried out, the field assay that sample is also able to achieve while greatly reducing analysis cost and detection immediately;3)
New method can directly be applied in the fields such as environmental monitoring, food safety, medical research Ag in various samples+Analyte or
Using the metal ion as the simple, economic, quick, special of other target analytes such as the protein of secondary analysis object, nucleic acid
Portable qualitative and quantitative detection, has broad application prospects.
Detailed description of the invention
Fig. 1 is the principle signal of the visual quantitative detecting method of simple silver ion in Example 1 and Example 2 of the present invention
Figure.
Marked in the figure: 1- cuvette;The scale of 2- cuvette outer wall;The colourless formamide solvent of 3-;4-3,3',5,
5'- tetramethyl benzidine solute;The colourless aqueous solvent of 5-;6-Ag+Solute;7- quinoid benzidine;8- contains the indigo plant of quinoid benzidine
Color solution;9- does not contain the colourless solution of quinoid benzidine;10- naked eyes.
Fig. 2 is that analysis 1mM contains Ag in the embodiment of the present invention 1+Aqueous solution when acquired results and blank sample (be free of Ag+
Ultrapure water) acquired results comparison figure.
Fig. 3 is dense using a series of differences of the visual quantitative detecting method analysis of simple silver ion in the embodiment of the present invention 2
The Ag of degree+Gained blue solution length (scale value on test tube outer wall) and Ag when aqueous solution+Log value (Log (the C of concentrationAg+))
Between working curve.
Specific embodiment
Following embodiment will be further described the present invention, but not thereby limiting the invention.
Embodiment 1:
The present embodiment contains Ag using the visual quantitative detecting method analysis 1mM of simple silver ion+Aqueous solution (A) and sky
White sample (is free of Ag+Ultrapure water, B).
Specific implementation process is as follows:
As shown in Figure 1, the specific steps of the present embodiment are as follows: step 1, by 50 μ L 1mM silver nitrate (AgNO3) water-soluble drop
Be added to equipped with 100 μ L 2.5mM TMB solution (by can miscible with water, 25 DEG C of lower densities be 1.134g/mL formamide prepare)
In the graduated plastic, transparent test tube of outer wall;Step 2, macroscopic visual observation, directly read it is long with blue solution in cuvette
Spend the scale on relevant cuvette outer wall, the size and Ag of the length+Concentration is positively correlated, i.e. completion Ag+It is visual quantitative
Detection.
Blank sample, i.e. ultrapure water (resistivity is 18.2M Ω cm) are tested and analyzed according to identical step, and is visually seen
Examine the color change of solution in test tube.Figure it is seen that is obtained when detection blank sample is colorless and transparent solution.This
It is because there is no Ag in blank sample+, so blue quinoid benzidine product does not generate.On the other hand, as detection 1mM
Contain Ag+Aqueous solution when, can obviously observe and form the colourless double-colored mixing of unique upper layer blue-lower layer in test tube
Solution.This is because working as Ag+When aqueous solution is added dropwise into TMB solution, the solute in two kinds of solution occurs a degree of
Exchange, Ag+Quickly oxidation TMB generates quinoid benzidine.Because the quinoid benzidine product is more likely to be formed in water phase, most
The colourless double-colored mixed solution of upper layer blue-lower layer is obtained eventually.Upper layer is mainly the lesser water phase of density, and because joining containing quinoid
Aniline product and blue is presented;Lower layer is mainly the biggish organic phase of density, and because not having quinoid benzidine product or the product
Concentration is too low and presents colourless.Contrast and experiment in Fig. 2 shows that the visual quantitative detecting method of silver ion is practical.
Embodiment 2:
The Ag that the present embodiment is 62.5 μM~4mM using the visual quantitative detecting method analytical concentration range of simple silver ion+Aqueous solution.
Specific implementation process is as follows:
As shown in Figure 1, detecting each Ag in the present embodiment+The specific steps of aqueous solution are as follows: step 1,50 μ L are a certain dense
Spend AgNO3Aqueous solution be added drop-wise to containing 100 μ L 2.5mM TMB solution (by can miscible with water, 25 DEG C of lower densities be 1.134g/mL
Formamide prepare) the graduated plastic, transparent test tube of outer wall in;Step 2, macroscopic visual observation, directly read with it is transparent
Scale in test tube on the relevant cuvette outer wall of blue solution length.By all Ag+The colored solutions length value of aqueous solution
(scale value i.e. on cuvette outer wall) is to Ag+Log value (Log (the C of concentrationAg+)) mapping (Fig. 3), i.e. completion Ag+It is visual
Quantitative detection.
From the figure 3, it may be seen that with Ag+The increase of concentration, the length value of blue solution is (i.e. outside cuvette in corresponding test tube
Scale value on wall) it is gradually increased.This is because working as Ag+When concentration is larger, the oxidable more TMB of the metal ion is generated
The blue quinoid benzidine product of larger concentration, directly performance are in test tube with the blue solution of larger lengths.In addition, Fig. 3
It has been shown that, the length value (scale value on cuvette outer wall) and Ag of blue solution+Log value (Log (the C of concentrationAg+))
Good linear relationship is presented within the scope of 62.5 μM~4mM.
Claims (1)
1. a kind of visual quantitative detecting method of simple silver ion, it is characterised in that specific steps are as follows:
Step 1 will contain Ag+Aqueous solution be added drop-wise to equipped with 3,3', in the cuvette of 5,5'- tetramethyl biphenyl amine aqueous solution;
Step 2, macroscopic visual observation, the length for measuring cuvette blue solution at the middle and upper levels, the size and Ag of the length+Concentration
It is positively correlated, i.e. completion Ag+Visual quantitative detection;
It is described to contain Ag+Aqueous solution in Ag+For target analytes or two fractions generated by chemical reaction and biological respinse
Analyse object;
The solvent of described 3,3', 5,5'- tetramethyl biphenyl amine aqueous solutions be organic solvent, the organic solvent it is miscible with water and 25 DEG C at
Density is greater than the density of water;
The cuvette is that the graduated cuvette of outer wall or outer wall do not have graduated cuvette, the material of cuvette
It is plastics or glass;When the outer wall of cuvette has scale, measuring cuvette, the length of blue solution is to pass through at the middle and upper levels
The scale on cuvette outer wall relevant to blue solution length is directly read to complete;When the outer wall of cuvette is not carved
When spending, measuring cuvette, the length of blue solution is measured in test tube on cuvette outer wall by using ruler at the middle and upper levels
The length of blue solution is completed.
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CN106932389A (en) * | 2017-03-28 | 2017-07-07 | 桂林理工大学 | Nm of gold Two-dimensional Liquid without spectrometer compares color quantitative analysis method |
CN108693175B (en) * | 2017-04-07 | 2021-07-30 | 南京大学 | Method for detecting copper ions by adopting high-throughput photoelectric colorimetric method |
CN109490384B (en) * | 2017-09-11 | 2021-04-02 | 中国科学院理化技术研究所 | Working electrode and electrochemical sensor for selectively detecting silver ions |
CN110243776A (en) * | 2019-06-21 | 2019-09-17 | 福建中医药大学 | Improve reaction microenvironment using lauryl sodium sulfate and carries out that silver ion is qualitative and the detection method of quantitative detection |
CN110579469B (en) * | 2019-09-29 | 2022-04-08 | 桂林理工大学 | Instrument-free quantitative detection method for divalent mercury ions |
CN112285099A (en) * | 2020-09-23 | 2021-01-29 | 嘉兴学院 | Visual hydrogel sensor and preparation method and application thereof |
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Application publication date: 20170222 Assignee: GUILIN VEIRUN MEDICAL TECHNOLOGY Co.,Ltd. Assignor: GUILIN University OF TECHNOLOGY Contract record no.: X2023980046003 Denomination of invention: A Simple Visual Quantitative Detection Method for Silver Ions Granted publication date: 20191011 License type: Common License Record date: 20231108 |
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